Investigation of the local mechanical properties of potassium chloride single crystals by atomic force microscopy

Using an atomic force microscope (AFM), the of hardness H and Young’s modulus E are measured in near-surface layers of KCl single crystals to a depth of 300 nm at loads of 5–100 µN. The values of H and E are estimated indirectly by analyzing P(h) curves (load vs. indentation depth curves). The value of H is also estimated directly by measuring the area of an indentation with the help of an AFM with a nanoscale resolution. The effect of structural features of the surface around an indentation on the accuracy of the H and E estimates is revealed. The sharp dependence of H on the load (the nanoscale effect) is revealed. The experimental results agree qualitatively with the predictions of the geometrically necessary dislocation model developed by Nix and Gao. However, in order to quantitatively estimate mass transfer from a nanoindenter, a structural analysis is required with allowance for plastic deformation in crystals.     

Calibrating a nanoindenter for very shallow depth indentation using equivalent contact radius

Nanoindenter tips are usually modelled as axisymmetric cones, with calibration involving finding a fitting function that relates contact area to contact depth. For accurate calibration of shallow depth indentation, this is not ideal because it means that deeper indents tend to dominate the fitting function. For an axisymmetric object, it is always possible to define an equivalent contact radius (which, in the case, of nanoindentation is linearly related to the reduced modulus) and to obtain a fitting function that relates this equivalent contact radius to indentation depth. The equivalent contact radius approach is used here to provide shallow depth calibration of a nanoindenter tip at three separate times. The advantage of the equivalent contact radius methodology is that it provides a clearer physical interpretation of the changes in tip shape than a conventional area-based fit. We also show that the minimum depth for a reliable hardness measurement is obtainable and increases as the tip blunts with age but that consistent measurements of very near surface elastic moduli can be made if the blunting of the tip over time is fully accounted for in the tip area function calibration.     

Nanomechanical characteristics of annealed Si/SiGe superlattices

In this study, the nanomechanical damage was investigated on the annealed Si/SiGe strained-layer superlattices (SLSs) deposited using an ultrahigh-vacuum chemical vapor deposition (UHVCVD). Nanoscratch, nanoindenter, atomic force microscopy (AFM), and transmission electron microscopy (TEM) techniques were used to determine the nanomechanical behavior of the SiGe films. With a constant force applied, greater hardness number and larger coefficients of friction (μ) were observed on the samples that had been annealed at 600 °C, suggesting that annealing of the Si/SiGe SLSs can induce greater shear resistance. AFM morphological studies of the Si/SiGe SLSs revealed that pile-up phenomena occurred on both sides of each scratch, with the formation of some pellets and microparticles. The Si/SiGe SLSs that had been subjected to annealing under various conditions exhibited significantly different features in their indentation results. Indeed, the TEM images reveal slight dislocation propagation in the microstructures. Thus, the hardness and elastic modulus can be increased slightly after annealing treatment because the existence of comparatively unstable microstructures. It is suggested that cracking phenomena dominate the damage cause of Si/SiGe SLSs.     

An international round-robin calibration protocol for nanoindentation measurements

Nanoindentation has become a common technique for measuring the hardness and elastic-plastic properties of materials, including coatings and thin films. In recent years, different nanoindenter instruments have been commercialised and used for this purpose. Each instrument is equipped with its own analysis software for the derivation of the hardness and reduced Young's modulus from the raw data. These data are mostly analysed through the Oliver and Pharr method. In all cases, the calibration of compliance and area function is mandatory. The present work illustrates and describes a calibration procedure and an approach to raw data analysis carried out for six different nanoindentation instruments through several round-robin experiments. Three different indenters were used, Berkovich, cube corner, spherical, and three standardised reference samples were chosen, hard fused quartz, soft polycarbonate, and sapphire. It was clearly shown that the use of these common procedures consistently limited the hardness and reduced the Young's modulus data spread compared to the same measurements performed using instrument-specific procedures. The following recommendations for nanoindentation calibration must be followed: (a) use only sharp indenters, (b) set an upper cut-off value for the penetration depth below which measurements must be considered unreliable, (c) perform nanoindentation measurements with limited thermal drift, (d) ensure that the load-displacement curves are as smooth as possible, (e) perform stiffness measurements specific to each instrument/indenter couple, (f) use Fq and Sa as calibration reference samples for stiffness and area function determination, (g) use a function, rather than a single value, for the stiffness and (h) adopt a unique protocol and software for raw data analysis in order to limit the data spread related to the instruments (i.e. the level of drift or noise, defects of a given probe) and to make the H and E(r) data intercomparable.     

Properties of Cu film and Ti/Cu film on polyimide prepared by ion beam techniques

Cu film and Ti/Cu film on polyimide substrate were prepared by ion implantation and ion beam assisted deposition (IBAD) techniques. Three-dimension white-light interfering profilometer was used to measure thickness of each film. The thickness of the Cu film and Ti/Cu film ranged between 490 nm and 640 nm. The depth profile, surface morphology, roughness, adhesion, nanohardness, and modulus of the Cu and Ti/Cu films were measured by scanning Auger nanoprobe (SAN), atomic force microscopy (AFM), and nanoindenter, respectively. The polyimide substrates irradiated with argon ions were analyzed by scanning electron microscopy (SEM) and AFM. The results suggested that both the Cu film and Ti/Cu film were of good adhesion with polyimide substrate, and ion beam techniques were suitable to prepare thin metal film on polyimide.     

Determination of silicone coating Young's modulus using atomic force microscopy

The polymerisation degree of thin polymer coatings was checked by following the variation of their local mechanical properties. Atomic force microscope (AFM) was used in an indentation mode to investigate the mechanical characteristics of silicone coatings on polycarbonate substrates. The evolution of Young's modulus of the silicone coatings was determined as a function of the polymer annealing time. We have used a relative method to measure Young's moduli, which involves a calibration step with a set of reference polymers. No variation was observed for the modulus of silicone coatings annealed during more than 40 min at 130 °C. This result indicates that over-heating does not modify the mechanical properties of the coating.     

Elastic modulus of suspended purple membrane measured by atomic force microscopy

We have probed the mechanical properties of purple membrane (PM) in a physiological environment using the atomic force microscope (AFM). By suspending PM over nano-trenches, the elastic properties of PM can be evaluated free from the interaction with the substrate. Force-displacement curves were obtained on the suspended membrane and the data was compared to that of a simple model of a thin film over a trench. By fitting the data to the model, the elastic modulus of PM was estimated to be 8 MPa. When the membrane is repeatedly indented, we observed a change in the force-distance data consistent with damage to the two-dimensional crystal of PM. In this paper we demonstrate that the AFM allows us to evaluate the mechanics of biological membranes in their native conditions.     

Elasticity and nanomechanical response of Aspergillus niger spores using atomic force microscopy

The elasticity and nanomechanical response of Aspergillus niger spores determined using atomic force microscopy (AFM) and nanoindentation are discussed. The force-displacement curve of the spore surfaces shows that the average surface roughness of spores was approximately 33 nm and that the adhesion force ranged from 9 to 28 nN. The Young's modulus of the A. niger spores ranged from 0.1 to 21.4 GPa and the hardness ranged from 0.01 to 0.17 GPa. The critical buckling load of the spore membrane is 290 μN.     

Effects of post-annealing on the structural and nanomechanical properties of Ga-doped ZnO thin films deposited on glass substrate by rf-magnetron sputtering

In this study, the effects of post-annealing on the structure, surface morphology and nanomechanical properties of ZnO thin films doped with a nominal concentration of 3 at.% Ga (ZnO:Ga) are investigated using X-ray diffraction (XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM) and nanoindentation techniques. The ZnO:Ga thin films were deposited on the glass substrates at room temperature by radio frequency magnetron sputtering. Results revealed that the as-deposited ZnO:Ga thin films were polycrystalline albeit the low deposition temperature. Post-annealing carried out at 300, 400 and 500 °C, respectively, has resulted in progressive increase in both the average grain size and the surface roughness of the ZnO:Ga thin film, in addition to the improved thin films crystallinity. Moreover, the hardness and Young's modulus of ZnO:Ga thin films are measured by a Berkovich nanoindenter operated with the continuous contact stiffness measurements (CSM) option. The hardness and Young's modulus of ZnO:Ga thin films increased as the annealing temperature increased from 300 to 500 °C, with the best results being obtained at 500 °C.     

Depth-dependent calibration for quantitative elemental depth profiling of copper alloys using laser-induced plasma spectroscopy

This work presents new calibration procedures for deep elemental depth profile analysis of bronze artifacts. A simple ablation model is developed for the estimation of the ablation rate and hence for deriving the depth spatial calibration scale. Elemental quantification is obtained through the construction of calibration surfaces, using reference samples of known composition, relating laser-induced plasma spectroscopy (LIPS) intensity ratios, content of atomic species and number of laser pulses. Such a method represents a refinement of the standard LIPS quantification approach based on calibration curves, which is extended here to the generation of significantly deep craters into the material under investigation up to several hundred microns. The depth dependence of the calibration surfaces measured is discussed in the framework of a simplified model of depth-dependent plasma temperature.     

Evaluation of nanoscale roughness measurements on a plasma treated SU-8 polymer surface by atomic force microscopy

A comparison between roughness data obtained with an atomic force microscope (AFM) on different surfaces requires reliable roughness parameters. In order to specify the appropriate parameters for nanoscale roughness measurements, we compared the root mean square (rms) roughness and the relative surface area (sdr) as function of varying scan size, speed and pixel size. By using oxygen plasma (24 kJ) treated SU-8 with an average rms roughness of 2.6 ± 0.5 nm as reference surface, the repeatability of the method was evaluated for dynamic (tapping) and contact mode. The evaluation of AFM images indicated a decrease of the effective tip radius after a few measurements. This degradation of the tip lowers the resolution of the image and can affect roughness measurements.     

Downwards to metrology in nanoscale: determination of the AFM tip shape with well-known sharp-edged calibration structures

More and more AFMs and AFM profilers will be used to quantify micro- and nanostructures. For a correct characterization and evaluation of the measured structural details, in the nanoscale range, knowledge of the current shape of the AFM tip is needed. Often, the interaction between the AFM tip and the sample leads to a change in the tip shape. Our concept for the determination of tip shapes is based on the measurement of a well-known sharp-edged silicon structure. Each calibration sample contains a selected structure serving as a calibrated width standard, and has a certified pitch. Consequently, the shape of AFM tips can be determined with an accuracy of 10 nm. Received: 2 September 2002 / Accepted: 2 September 2002 / Published online: 5 March 2003 RID="*" ID="*"Corresponding author. Fax: +49-3641/206-199, E-mail: huebner@ipht-jena.de     

A convenient method to determine the bulk modulus of nanowires and its temperature dependence based on X-ray diffraction measurement

The bulk modulus of nanowires (NWs) and its temperature dependence were determined by a simple and convenient method based on temperature-dependent X-ray diffraction (XRD) measurement. It was found that the bulk moduli for Ni, Cu, and Ag NWs were much higher than that for their counterpart bulk materials in the temperature range from 25 °C to 800 °C and the influence of temperature on the bulk modulus for NWs was stronger than that for their counterpart bulk materials. A surface bond contraction model and the force–interatomic-distance curves were introduced to explain the experimental results.     

A universal DC characterisation system for hard and soft magnetic materials

A fully automatic system has been designed for the accurate measurement of the DC magnetic properties of soft and hard ferromagnetic materials utilising discrete calibrated instruments in order to provide a traceable calibration route separate from the transfer of standard magnetic test samples. Custom written software is used to operate the system in one of three modes, constant dH/dt, variable dH/dt and a second quadrant demagnetisation curve mode. The first two of these modes are utilised for soft magnetic materials with the second mode varying dH/dt in order to keep dB/dt relatively constant. Both modes use cycle times of between 60 and 300 s and may utilise a variety of test configurations including a bar permeameter, electromagnet, ring samples or Epstein frame. The minimum cycle time and the most appropriate mode is dependent on the particular sample and the effect of this on materials with a large dB/dH is significant. Measurements on soft materials include major BH loop, minor BH loops, first-order reversal curves, remanence, coercivity, normal magnetisation curve, peak permeability and loop area. The third mode is used with an electromagnet to measure the demagnetisation curve of hard magnetic materials up to a maximum demagnetisation field of 1.6 MA/m. The measurement algorithm modulates dH/dt depending on dB/dt and incorporates holdback in order to accommodate rare earth materials which exhibit high viscosity.     

Electrostatic and van der Waals forces in the air contact between the atomic force microscope probe and a conducting surface

Electrostatic and van der Waals forces of interaction between commercial probes of atomic force microscopes (AFMs) and conducting surfaces under atmospheric conditions are measured using contact atomic force microscopy. An algorithm of statistical processing of the initial photocurrent-displacement dependences is developed, which makes it possible to transform these dependences into the force-distance dependences. The Hamaker constant at the platinum (probe)-graphite (sample) contact is determined. It is shown that the measurement of electrostatic forces makes it possible to determine geometrical parameters of the AFM probe and to independently calibrate the stiffness of the cantilever.     

Quantitative imaging of electrospun fibers by PeakForce Quantitative NanoMechanics atomic force microscopy using etched scanning probes

Electrospun polymeric submicron and nanofibers can be used as tissue engineering scaffolds in regenerative medicine. In physiological conditions fibers are subjected to stresses and strains from the surrounding biological environment. Such stresses can cause permanent deformation or even failure to their structure. Therefore, there is a growing necessity to characterize their mechanical properties, especially at the nanoscale.Atomic force microscopy is a powerful tool for the visualization and probing of selected mechanical properties of materials in biomedical sciences. Image resolution of atomic force microscopy techniques depends on the equipment quality and shape of the scanning probe. The probe radius and aspect ratio has huge impact on the quality of measurement.In the presented work the nanomechanical properties of four different polymer based electrospun fibers were tested using PeakForce Quantitative NanoMechanics atomic force microscopy, with standard and modified scanning probes. Standard, commercially available probes have been modified by etching using focused ion beam (FIB). Results have shown that modified probes can be used for mechanical properties mapping of biomaterial in the nanoscale, and generate nanomechanical information where conventional tips fail.     

Ultrasound enhanced the binding ability of chitinase onto chitin: From an AFM insight

In order to evaluate the effect of ultrasound to chitinase from a molecular level, atomic force microscopy (AFM) was employed to investigate the interaction force of chitinase binding onto chitin surface. In the measurement of force-distance curve, a series of pull-off events were discovered using the immobilized AFM tips with chitinase either treated by ultrasound or not, whereas no interaction peak was observed by the AFM tips without chitinase, indicating that the obtained adhesion forces were coming from the binding functions between chitinase and chitin. Through the analysis of these force curves, at the loading velocity of 0.3 μm/s, the maximum binding force of the chitinase treated by ultrasound for 20 min onto chitin was measured to be 105.33 ± 23.51 pN, while the untreated onto chitin was 71.05 ± 12.73 pN, suggesting the stronger binding force between ultrasonic treated chitinase and chitin substrate. Therefore, AFM has provided a useful method to directly and quantitatively characterize the interactions between chitinase and chitin, and successfully proved that ultrasound could activate chitinase by enhancing the binding ability of chitinase onto chitin.     

Tribological properties of silicate materials on nano and microscale

We studied the friction properties of four model silicate materials at the nanoscale and microscale. From nanotribology, we characterized the tribological properties at single asperity contact scale and from microtribology, we characterized the tribological properties at multi asperity contact scale. First, for each material we measured chemical composition by XPS, Young's modulus by acoustical microscopy and roughness σ by atomic force microscopy (AFM). Second, we measured the nanofriction coefficients with an AFM and the microfriction coefficients with a ball probe tribometer, for three hardnesses of the ball probe. We identified one friction mechanism at the nanoscale (sliding friction) and two friction mechanisms at the microscale (sliding friction and yielding friction). Comparison of the nano and microfriction coefficients at the same sliding friction regime shown, that the tribological properties of these materials didn’t depend on roughness.     

The formation of sub-10 nm nanohole array on block copolymer thin films on gold surface using surface neutralization based on O2 plasma treatment and self-assembled monolayer

Blockcopolymer (BCP) lithography is an emerging nanolithography technique for fabrications of various nanoscale devices and materials. In this study, self-assembled BCP thin films having cylindrical nanoholes were prepared on gold by surface neutralization using self-assembled monolayer (SAM). Oxygen plasma treatment was investigated as a way to enhance the functionality of Au surface toward SAM formation. After surface neutralization, well-ordered nanoholes with 9 to 20 nm diameters were formed inside BCP thin films on Au surfaces through microphase separation. The effects of oxygen plasma treatment on the formation of BCP nanopattern were investigated using surface analysis techniques including X-ray photoelectron spectroscopy (XPS) and water contact angle measurement. Au nanodot arrays were fabricated on gold film by utilizing the BCP nanotemplate and investigated by atomic force microscopy (AFM).     

Nanoindentation of gold nanoparticles functionalized with proteins

The hardness and Young's modulus of 10 and 20 nm gold nanoparticles (Au NPs) modified with bovine serum albumin and streptavidin were measured using a nanoindenter. The Au NPs were immobilized on a semiconductor surface through organic self-assembled monolayers. Changes in mechanical properties occurred when the Au NPs were immobilized on the surface. The hardness and Young's modulus were dependent on the size of the NPs, and the proteins on the particles showed highly plastic and elastic behavior compared to flat surfaces modified with self-assembled monolayers.