Special Issue "Small Scale Deformation using Advanced Nanoindentation Techniques"

A special issue of Micromachines (ISSN 2072-666X). This special issue belongs to the section "D:Materials and Processing".

Deadline for manuscript submissions: closed (15 October 2018)

Printed Edition Available!
A printed edition of this Special Issue is available here.

Special Issue Editors

Guest Editor
Prof. Dr. Ting Tsui

Department of Chemical Engineering, University of Waterloo, 200 University Avenue West, Waterloo, ON N2L 3G1, Canada
Website | E-Mail
Interests: nanoindentation; sub-micron fabrication; nanomechanics; thin film delaminations; integrate circuits; cell immobilization; morphology control of cells
Guest Editor
Prof. Dr. Alex A. Volinsky

Department of Mechanical Engineering, University of South Florida, 4202 E Fowler Ave. ENB 118 Tampa, FL 33620, USA
Website | E-Mail
Phone: 8139745658
Interests: thin films processing; mechanical properties and characterization; adhesion and fracture of thin films; nanoindentation; pattern formation; irradiated materials properties; X-Ray diffraction

Special Issue Information

Dear Colleagues,

Small scale mechanical deformations have gained a significant interest over the past few decades, driven by the advances in integrated circuits and microelectromechanical systems. One of the most powerful and versatile characterization methods is the nanoindentation technique. The capabilities of these depth-sensing instruments have been improved considerably. They can perform experiments in vacuum and at high temperatures, such as in-situ SEM and TEM nanoindenters. This allows researchers to visualize mechanical deformations and dislocations motion in real time. Time-dependent behavior of soft materials has also been studied in recent research works. This Special Issue on "Small Scale Deformation using Advanced Nanoindentation Techniques"; will provide a forum for researchers from the academic and industrial communities to present advances in the field of small scale contact mechanics. Materials of interest include metals, glass, and ceramics. Manuscripts related to deformations of biomaterials and biological related specimens are also welcome. Topics of interest include, but are not limited to:

  • Small scale facture
  • Nanoscale plasticity and creep
  • Size-dependent deformation phenomena
  • Deformation of biological cells
  • Mechanical properties of cellular and sub-cellular components
  • Novel mechanical properties characterization techniques
  • New modeling methods
  • Environmentally controlled nanoindentation
  • In-situ SEM and TEM indentation

Prof. Dr. Ting Tsui
Prof. Dr. Alex A. Volinsky
Guest Editors

Manuscript Submission Information

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Keywords

  • Nanoindentation
  • Small scale mechanical properties
  • Deformation
  • Cells
  • Plasticity
  • Fracture
  • Contact mechanics

Published Papers (12 papers)

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Editorial

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Open AccessEditorial
Editorial for the Special Issue on Small-Scale Deformation using Advanced Nanoindentation Techniques
Micromachines 2019, 10(4), 269; https://doi.org/10.3390/mi10040269
Received: 14 April 2019 / Accepted: 16 April 2019 / Published: 22 April 2019
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Abstract
Nanoindentation techniques have been used to reliably characterize mechanical properties at small scales for the past 30 years [...] Full article

Research

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Open AccessCommunication
The Impact of Hydrogen on Mechanical Properties; A New In Situ Nanoindentation Testing Method
Micromachines 2019, 10(2), 114; https://doi.org/10.3390/mi10020114
Received: 13 January 2019 / Revised: 4 February 2019 / Accepted: 6 February 2019 / Published: 11 February 2019
Cited by 1 | PDF Full-text (1304 KB) | HTML Full-text | XML Full-text
Abstract
We have designed a new method for electrochemical hydrogen charging which allows us to charge very thin coarse-grained specimens from the bottom and perform nanomechanical testing on the top. As the average grain diameter is larger than the thickness of the sample, this [...] Read more.
We have designed a new method for electrochemical hydrogen charging which allows us to charge very thin coarse-grained specimens from the bottom and perform nanomechanical testing on the top. As the average grain diameter is larger than the thickness of the sample, this setup allows us to efficiently evaluate the mechanical properties of multiple single crystals with similar electrochemical conditions. Another important advantage is that the top surface is not affected by corrosion by the electrolyte. The nanoindentation results show that hydrogen reduces the activation energy for homogenous dislocation nucleation by approximately 15–20% in a (001) grain. The elastic modulus also was observed to be reduced by the same amount. The hardness increased by approximately 4%, as determined by load-displacement curves and residual imprint analysis. Full article
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Open AccessArticle
In Situ Mechanical Characterization of the Mixed-Mode Fracture Strength of the Cu/Si Interface for TSV Structures
Micromachines 2019, 10(2), 86; https://doi.org/10.3390/mi10020086
Received: 7 December 2018 / Revised: 17 January 2019 / Accepted: 21 January 2019 / Published: 25 January 2019
Cited by 1 | PDF Full-text (4487 KB) | HTML Full-text | XML Full-text
Abstract
In situ nanoindentation experiments have been widely adopted to characterize material behaviors of microelectronic devices. This work introduces the latest developments of nanoindentation experiments in the characterization of nonlinear material properties of 3D integrated microelectronic devices using the through-silicon via (TSV) technique. The [...] Read more.
In situ nanoindentation experiments have been widely adopted to characterize material behaviors of microelectronic devices. This work introduces the latest developments of nanoindentation experiments in the characterization of nonlinear material properties of 3D integrated microelectronic devices using the through-silicon via (TSV) technique. The elastic, plastic, and interfacial fracture behavior of the copper via and matrix via interface were characterized using small-scale specimens prepared with a focused ion beam (FIB) and nanoindentation experiments. A brittle interfacial fracture was found at the Cu/Si interface under mixed-mode loading with a phase angle ranging from 16.7° to 83.7°. The mixed-mode fracture strengths were extracted using the linear elastic fracture mechanics (LEFM) analysis and a fracture criterion was obtained by fitting the extracted data with the power-law function. The vectorial interfacial strength and toughness were found to be independent with the mode-mix. Full article
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Open AccessArticle
Testing Effects on Shear Transformation Zone Size of Metallic Glassy Films Under Nanoindentation
Micromachines 2018, 9(12), 636; https://doi.org/10.3390/mi9120636
Received: 22 October 2018 / Revised: 19 November 2018 / Accepted: 28 November 2018 / Published: 30 November 2018
Cited by 3 | PDF Full-text (4734 KB) | HTML Full-text | XML Full-text
Abstract
Room-temperature creep tests are performed at the plastic regions of two different metallic glassy films under Berkovich nanoindetation. Relying on the strain rate sensitivity of the steady-state creep curve, shear transformation zone (STZ) size is estimated based on the cooperative shear model (CSM). [...] Read more.
Room-temperature creep tests are performed at the plastic regions of two different metallic glassy films under Berkovich nanoindetation. Relying on the strain rate sensitivity of the steady-state creep curve, shear transformation zone (STZ) size is estimated based on the cooperative shear model (CSM). By applying various indentation depths, loading rates, and holding times, the testing effects on the STZ size of metallic glasses are systematically studied. Experimental results indicate that STZ size is greatly increased with increased indentation depth and shortened holding time. Meanwhile, STZ size is weakly dependent on the loading history. Both the intrinsic and extrinsic reasons are discussed, to reveal the testing effects on the nanoindentation creep flow and STZ size. Full article
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Open AccessArticle
Nanoindentation and TEM to Study the Cavity Fate after Post-Irradiation Annealing of He Implanted EUROFER97 and EU-ODS EUROFER
Micromachines 2018, 9(12), 633; https://doi.org/10.3390/mi9120633
Received: 25 October 2018 / Revised: 22 November 2018 / Accepted: 23 November 2018 / Published: 29 November 2018
Cited by 2 | PDF Full-text (9489 KB) | HTML Full-text | XML Full-text
Abstract
The effect of post-helium irradiation annealing on bubbles and nanoindentation hardness of two reduced activation ferritic martensitic steels for nuclear fusion applications (EUROFER97 and EU-ODS EUROFER) has been studied. Helium-irradiated EUROFER97 and EU-ODS EUROFER were annealed at 450 °C for 100 h in [...] Read more.
The effect of post-helium irradiation annealing on bubbles and nanoindentation hardness of two reduced activation ferritic martensitic steels for nuclear fusion applications (EUROFER97 and EU-ODS EUROFER) has been studied. Helium-irradiated EUROFER97 and EU-ODS EUROFER were annealed at 450 °C for 100 h in an argon atmosphere. The samples were tested by nanoindentation and studied by transmission electron microscopy extracting some focused ion beam lamellae containing the whole implanted zone (≈50 µm). A substantial increment in nanoindentation hardness was measured in the area with higher helium content, which was larger in the case of EUROFER97 than in EU-ODS EUROFER. In terms of microstructure defects, while EU-ODS EUROFER showed larger helium bubbles, EUROFER97 experienced the formation of a great population density of them, which means that the mechanism that condition the evolution of cavities for these two materials are different and completely dependent on the microstructure. Full article
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Open AccessArticle
Static and Fatigue Tests on Cementitious Cantilever Beams Using Nanoindenter
Micromachines 2018, 9(12), 630; https://doi.org/10.3390/mi9120630
Received: 2 November 2018 / Revised: 15 November 2018 / Accepted: 22 November 2018 / Published: 28 November 2018
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Abstract
Cement paste is the main binding component in concrete and thus its fundamental properties are of great significance for understanding the fracture behaviour as well as the ageing process of concrete. One major aim of this paper is to characterize the micromechanical properties [...] Read more.
Cement paste is the main binding component in concrete and thus its fundamental properties are of great significance for understanding the fracture behaviour as well as the ageing process of concrete. One major aim of this paper is to characterize the micromechanical properties of cement paste with the aid of a nanoindenter. Besides, this paper also presents a preliminary study on the fatigue behaviour of cement paste at the micrometer level. Miniaturized cantilever beams made of cement paste with different water/cement ratios were statically and cyclically loaded. The micromechanical properties of cement paste were determined based on the measured load-displacement curves. The evolution of fatigue damage was evaluated in terms of the residual displacement, strength, and elastic modulus. The results show that the developed test procedure in this work is able to produce reliable micromechanical properties of cement paste. In addition, little damage was observed in the cantilever beams under the applied stress level of 50% to 70% for 1000 loading cycles. This work may shed some light on studying the fatigue behaviour of concrete in a multiscale manner. Full article
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Open AccessArticle
Localized Deformation and Fracture Behaviors in InP Single Crystals by Indentation
Micromachines 2018, 9(12), 611; https://doi.org/10.3390/mi9120611
Received: 11 October 2018 / Revised: 14 November 2018 / Accepted: 18 November 2018 / Published: 22 November 2018
Cited by 2 | PDF Full-text (1747 KB) | HTML Full-text | XML Full-text
Abstract
The indentation-induced deformation mechanisms in InP(100) single crystals were investigated by using nanoindentation and cross-sectional transmission electron microscopy (XTEM) techniques. The results indicated that there were multiple “pop-in” events randomly distributed in the loading curves, which were conceived to arise primarily from the [...] Read more.
The indentation-induced deformation mechanisms in InP(100) single crystals were investigated by using nanoindentation and cross-sectional transmission electron microscopy (XTEM) techniques. The results indicated that there were multiple “pop-in” events randomly distributed in the loading curves, which were conceived to arise primarily from the dislocation nucleation and propagation activities. An energetic estimation on the number of nanoindentation-induced dislocations associated with pop-in effects is discussed. Furthermore, the fracture patterns were performed by Vickers indentation. The fracture toughness and the fracture energy of InP(100) single crystals were calculated to be around 1.2 MPa·m1/2 and 14.1 J/m2, respectively. Full article
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Open AccessArticle
Calibration of a Constitutive Model from Tension and Nanoindentation for Lead-Free Solder
Micromachines 2018, 9(11), 608; https://doi.org/10.3390/mi9110608
Received: 5 October 2018 / Revised: 9 November 2018 / Accepted: 14 November 2018 / Published: 20 November 2018
Cited by 1 | PDF Full-text (6447 KB) | HTML Full-text | XML Full-text
Abstract
It is challenging to evaluate constitutive behaviour by using conventional uniaxial tests for materials with limited sizes, considering the miniaturization trend of integrated circuits in electronic devices. An instrumented nanoindentation approach is appealing to obtain local properties as the function of penetration depth. [...] Read more.
It is challenging to evaluate constitutive behaviour by using conventional uniaxial tests for materials with limited sizes, considering the miniaturization trend of integrated circuits in electronic devices. An instrumented nanoindentation approach is appealing to obtain local properties as the function of penetration depth. In this paper, both conventional tensile and nanoindentation experiments are performed on samples of a lead-free Sn–3.0Ag–0.5Cu (SAC305) solder alloy. In order to align the material behaviour, thermal treatments were performed at different temperatures and durations for all specimens, for both tensile experiments and nanoindentation experiments. Based on the self-similarity of the used Berkovich indenter, a power-law model is adopted to describe the stress–strain relationship by means of analytical dimensionless analysis on the applied load-penetration depth responses from nanoindentation experiments. In light of the significant difference of applied strain rates in the tensile and nanoindentation experiments, two “rate factors” are proposed by multiplying the representative stress and stress exponent in the adopted analytical model, and the corresponding values are determined for the best predictions of nanoindentation responses in the form of an applied load–indentation depth relationship. Eventually, good agreement is achieved when comparing the stress–strain responses measured from tensile experiments and estimated from the applied load–indentation depth responses of nanoindentation experiments. The rate factors ψ σ and ψ n are calibrated to be about 0.52 and 0.10, respectively, which facilitate the conversion of constitutive behaviour from nanoindentation experiments for material sample with a limited size. Full article
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Open AccessArticle
Nanoindentation of Bi2Se3 Thin Films
Micromachines 2018, 9(10), 518; https://doi.org/10.3390/mi9100518
Received: 21 August 2018 / Revised: 6 October 2018 / Accepted: 12 October 2018 / Published: 14 October 2018
Cited by 4 | PDF Full-text (2715 KB) | HTML Full-text | XML Full-text
Abstract
The nanomechanical properties and nanoindentation responses of bismuth selenide (Bi2Se3) thin films are investigated in this study. The Bi2Se3 thin films are deposited on c-plane sapphire substrates using pulsed laser deposition. The microstructural properties of [...] Read more.
The nanomechanical properties and nanoindentation responses of bismuth selenide (Bi2Se3) thin films are investigated in this study. The Bi2Se3 thin films are deposited on c-plane sapphire substrates using pulsed laser deposition. The microstructural properties of Bi2Se3 thin films are analyzed by means of X-ray diffraction (XRD). The XRD results indicated that Bi2Se3 thin films are exhibited the hexagonal crystal structure with a c-axis preferred growth orientation. Nanoindentation results showed the multiple “pop-ins” displayed in the loading segments of the load-displacement curves, suggesting that the deformation mechanisms in the hexagonal-structured Bi2Se3 films might have been governed by the nucleation and propagation of dislocations. Further, an energetic estimation of nanoindentation-induced dislocation associated with the observed pop-in effects was made using the classical dislocation theory. Full article
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Open AccessArticle
Nanoscale-Textured Tantalum Surfaces for Mammalian Cell Alignment
Micromachines 2018, 9(9), 464; https://doi.org/10.3390/mi9090464
Received: 12 July 2018 / Revised: 7 September 2018 / Accepted: 10 September 2018 / Published: 13 September 2018
Cited by 2 | PDF Full-text (9007 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
Tantalum is one of the most important biomaterials used for surgical implant devices. However, little knowledge exists about how nanoscale-textured tantalum surfaces affect cell morphology. Mammalian (Vero) cell morphology on tantalum-coated comb structures was studied using high-resolution scanning electron microscopy and fluorescence microscopy. [...] Read more.
Tantalum is one of the most important biomaterials used for surgical implant devices. However, little knowledge exists about how nanoscale-textured tantalum surfaces affect cell morphology. Mammalian (Vero) cell morphology on tantalum-coated comb structures was studied using high-resolution scanning electron microscopy and fluorescence microscopy. These structures contained parallel lines and trenches with equal widths in the range of 0.18 to 100 μm. Results showed that as much as 77% of adherent cell nuclei oriented within 10° of the line axes when deposited on comb structures with widths smaller than 10 μm. However, less than 20% of cells exhibited the same alignment performance on blanket tantalum films or structures with line widths larger than 50 μm. Two types of line-width-dependent cell morphology were observed. When line widths were smaller than 0.5 μm, nanometer-scale pseudopodia bridged across trench gaps without contacting the bottom surfaces. In contrast, pseudopodia structures covered the entire trench sidewalls and the trench bottom surfaces of comb structures with line-widths larger than 0.5 μm. Furthermore, results showed that when a single cell simultaneously adhered to multiple surface structures, the portion of the cell contacting each surface reflected the type of morphology observed for cells individually contacting the surfaces. Full article
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Open AccessArticle
Multiscale Analysis of Size Effect of Surface Pit Defect in Nanoindentation
Micromachines 2018, 9(6), 298; https://doi.org/10.3390/mi9060298
Received: 24 May 2018 / Revised: 4 June 2018 / Accepted: 10 June 2018 / Published: 13 June 2018
Cited by 3 | PDF Full-text (4852 KB) | HTML Full-text | XML Full-text
Abstract
The nanoindentation on a pit surface has been simulated using the quasicontinuum method in order to investigate the size effect of surface pit defect on the yield load of thin film. Various widths and heights of surface pit defect have been taken into [...] Read more.
The nanoindentation on a pit surface has been simulated using the quasicontinuum method in order to investigate the size effect of surface pit defect on the yield load of thin film. Various widths and heights of surface pit defect have been taken into account. The size coefficient has been defined as an index to express the influence of the width or height of surface pit defect. The results show that as the size coefficient of width (of height) increases, at first the yield load of thin film decreases extremely slowly, until the size coefficient of width equals approximately one unit (half unit), at which point the yield load experiences an obvious drop. When the size coefficient of width (of height) reaches approximately two units (one unit), the yield load is almost the same as that of the nanoindentation on a stepped surface. In addition, the height of surface pit defect has more influence than the width on the yield load of thin film. Full article
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Review

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Open AccessReview
Nanoindentation of Soft Biological Materials
Micromachines 2018, 9(12), 654; https://doi.org/10.3390/mi9120654
Received: 29 October 2018 / Revised: 27 November 2018 / Accepted: 5 December 2018 / Published: 11 December 2018
Cited by 3 | PDF Full-text (2909 KB) | HTML Full-text | XML Full-text
Abstract
Nanoindentation techniques, with high spatial resolution and force sensitivity, have recently been moved into the center of the spotlight for measuring the mechanical properties of biomaterials, especially bridging the scales from the molecular via the cellular and tissue all the way to the [...] Read more.
Nanoindentation techniques, with high spatial resolution and force sensitivity, have recently been moved into the center of the spotlight for measuring the mechanical properties of biomaterials, especially bridging the scales from the molecular via the cellular and tissue all the way to the organ level, whereas characterizing soft biomaterials, especially down to biomolecules, is fraught with more pitfalls compared with the hard biomaterials. In this review we detail the constitutive behavior of soft biomaterials under nanoindentation (including AFM) and present the characteristics of experimental aspects in detail, such as the adaption of instrumentation and indentation response of soft biomaterials. We further show some applications, and discuss the challenges and perspectives related to nanoindentation of soft biomaterials, a technique that can pinpoint the mechanical properties of soft biomaterials for the scale-span is far-reaching for understanding biomechanics and mechanobiology. Full article
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