Design and Evaluation of Torsional Probes for Multifrequency Atomic Force Microscopy

Multifrequency atomic force microscopy is a powerful nanoscale imaging and characterization technique that involves excitation of the atomic force microscope (AFM) probe and measurement of its response at multiple frequencies. This paper reports the design, fabrication, and evaluation of AFM probes with a specified set of torsional eigen-frequencies that facilitate enhancement of sensitivity in multifrequency AFM. A general approach is proposed to design the probes, which includes the design of their generic geometry, adoption of a simple lumped-parameter model, guidelines for determination of the initial dimensions, and an iterative scheme to obtain a probe with the specified eigen-frequencies. The proposed approach is employed to design a harmonic probe wherein the second and the third eigen-frequencies are the corresponding harmonics of the first eigen-frequency. The probe is subsequently fabricated and evaluated. The experimentally evaluated eigen-frequencies and associated mode shapes are shown to closely match the theoretical results. Finally, a simulation study is performed to demonstrate significant improvements in sensitivity to the second-and the third-harmonic spectral components of the tip-sample interaction force with the harmonic probe compared to that of a conventional probe.

Combined Atomic Force Microscopy and Modeling Study of The Evolution of Octadecylamine Films on a Mica Surface

The time evolution of the film thickness and domain formation of octadecylamine molecules adsorbed oil a mica surface is investigated Using atomic force microscopy. The adsorbed Film thickness is determined by measuring the height profile across the mica-amine interface of a mica surface partially immersed in a 15 mM solution of octadecylamine in chloroform. Using this novel procedure, adsorption of amine on mica is found to occur in three distinct stages, with morphologically distinct domain Formation and growth occurring during each stage. In the first stage, where adsorption is primarily in the thin-film regime, all average Film thickness of 0.2 (+/- 0.3) nm is formed for exposure times below 30 s and 0.8 (+/- 0.2) nm for 60 s of immersion time. During this stage, large sample spanning domains are observed. The second stage, which occurs between 60-300 s, is associated with it regime of rapid film growth, and the film thickness increases from about 0.8 to 25 nm during this stage. Once the thick-film regime is established, further exposure to the amine solution results in all increase in the domain area, and it regime of lateral domain growth is observed. In this stage, the domain area coverage grows from 38 to 75%, and the FTIR spectra reveal an increased level of crystallinity in the film. Using it diffusion-controlled model and it two-step Langmuir isotherm, the time evolution of the film growth is quantitatively captured. The model predicts the time at which the thin to thick film transition occurs as well its the time required for complete film growth at longer times. The Ward-Tordai equation is also solved to determine the model parameters in the monolayer (thin-film) regime, which occurs during the initial stages of film growth.

Measurement of Electron Spin Lifetime and Optical Orientation Efficiency in Germanium Using Electrical Detection of Radio Frequency Modulated Spin Polarization

We propose and demonstrate a technique for electrical detection of polarized spins in semiconductors in zero applied magnetic fields. Spin polarization is generated by optical injection using circularly polarized light which is modulated rapidly using an electro-optic cell. The modulated spin polarization generates a weak time-varying magnetic field which is detected by a sensitive radio-frequency coil. Using a calibrated pickup coil and amplification electronics, clear signals were obtained for bulk GaAs and Ge samples from which an optical spin orientation efficiency of 4.8% could be determined for Ge at 1342 nm excitation wavelength. In the presence of a small external magnetic field, the signal decayed according to the Hanle effect, from which a spin lifetime of 4.6 +/- 1.0 ns for electrons in bulk Ge at 127 K was extracted.

Enhanced endocytosis of nano-curcumin in nasopharyngeal cancer cells: An atomic force microscopy study

Recent studies in drug development have shown that curcumin can be a good competent due to its improved anticancer, antioxidant, anti-proliferative, and anti-inflammatory activities. A detailed real time characterization of drug (curcumin)-cell interaction is carried out in human nasopharyngeal cancer cells using atomic force microscopy. Nanocurcumin shows an enhanced uptake over micron sized drugs attributed to the receptor mediated route. Cell membrane stiffness plays a critical role in the drug endocytosis in nasopharyngeal cancer cells. (C) 2011 American Institute of Physics. [doi:10.1063/1.3653388]

High sensitivity detection of radio-frequency modulated magnetic moment in semiconductors

An experimental setup has been realized to measure weak magnetic moments which can be modulated at radio frequencies (similar to 1-5 MHz). Using an optimized radio-frequency (RF) pickup coil and lock-in amplifier, an experimental sensitivity of 10(-15) Am(2) corresponding to 10(-18) emu has been demonstrated with a 1 s time constant. The detection limit at room temperature is 9.3 x 10(-16) Am(2)/root Hz limited by Johnson noise of the coil. The setup has been used to directly measure the magnetic moment due to a small number (similar to 7 x 10(8)) of spin polarized electrons generated by polarization modulated optical radiation in GaAs and Ge. (C) 2011 American Institute of Physics. [doi: 10.1063/1.3654229]

Note: Design and development of an integrated three-dimensional scanner for atomic force microscopy

A compact scanning head for the Atomic Force Microscope (AFM) greatly enhances the portability of AFM and facilitates easy integration with other tools. This paper reports the design and development of a three-dimensional (3D) scanner integrated into an AFM micro-probe. The scanner is realized by means of a novel design for the AFM probe along with a magnetic actuation system. The integrated scanner, the actuation system, and their associated mechanical mounts are fabricated and evaluated. The experimentally calibrated actuation ranges are shown to be over 1 mu m along all the three axes. (c) 2013 AIP Publishing LLC.

Direct Measurement of Three-Dimensional Forces in Atomic Force Microscopy

Direct measurement of three-dimensional (3-D) forces between an atomic force microscope (AFM) probe and the sample benefits diverse applications of AFM, including force spectroscopy, nanometrology, and manipulation. This paper presents the design and evaluation of a measurement system, wherein the deflection of the AFM probe is obtained at two points to enable direct measurement of all the three components of 3-D tip-sample forces in real time. The optimal locations for measurement of deflection on the probe are derived for a conventional AFM probe. Further, a new optimal geometry is proposed for the probe that enables measurement of 3-D forces with identical sensitivity and nearly identical resolution along all three axes. Subsequently, the designed measurement system and the optimized AFM probe are both fabricated and evaluated. The evaluation demonstrates accurate measurement of tip-sample forces with minimal cross-sensitivities. Finally, the real-time measurement system is employed as part of a feedback control system to regulate the normal component of the interaction force, and to perform force-controlled scribing of a groove on the surface of polymethyl methacrylate.

Quantitative characterization of adhesion and stiffness of corneal lens of Drosophila melanogaster using atomic force microscopy

Atomic force Microscopy (AFM) has become a versatile tool in biology due to its advantage of high-resolution imaging of biological samples close to their native condition. Apart from imaging, AFM can also measure the local mechanical properties of the surfaces. In this study, we explore the possibility of using AFM to quantify the rough eye phenotype of Drosophila melanogaster through mechanical properties. We have measured adhesion force, stiffness and elastic modulus of the corneal lens using AFM. Various parameters affecting these measurements like cantilever stiffness and tip geometry are systematically studied and the measurement procedures are standardized. Results show that the mean adhesion force of the ommatidial surface varies from 36 nN to 16 nN based on the location. The mean stiffness is 483 +/- 5 N/m, and the elastic modulus is 3.4 +/- 0.05 GPa (95% confidence level) at the center of ommatidia. These properties are found to be different in corneal lens of eye expressing human mutant tau gene (mutant). The adhesion force, stiffness and elastic modulus are decreased in the mutant. We conclude that the measurement of surface and mechanical properties of D. melanogaster using AFM can be used for quantitative evaluation of `rough eye' surface. (C) 2015 Elsevier Ltd. All rights reserved.

Nano-meter scale plasticity in KBr studied by nanoindenter and force microscopy

The early stages of plasticity in KBr single crystals have been studied by means of nano-meter-scale indentation in complementary experiments using both a nanoindenter and an atomic force microscope. Nanoindentafion experiments precisely correlate indentation depth and forces, while force microscopy provides high-resolution force measurements and images of the surface revealing dislocation activity. The two methods provide very similar results for the onset of plasticity in KBr. Upon loading we observe yield of the surface in atomic layer units which we attribute to the nucleation of single dislocations. Unloading is accompanied by plastic recovery as evident from a non-linear force distance unloading curve and delayed discrete plasticity events.

Electrical and structural properties of zirconia thin films prepared by reactive magnetron sputtering

Thin films of ZrO2 were prepared by reactive magnetron sputtering. Annealing of the films exhibited a drastic change in the properties due to improved crystallinity and packing density. The root mean square roughness of the sample observed from atomic force microscope is about 5.75 nm which is comparable to the average grain size of the thin film which is about 6 nm obtained from X-ray diffraction. The film annealed at 873 K exhibits an optical band gap of around 4.83 eV and shows +4 oxidation state of zirconium indicating fully oxidized zirconium, whereas higher annealing temperatures lead to oxygen deficiency in the films and this is reflected in their properties. A discontinuity in the imaginary part of the AC conductivity was observed in the frequency range of tens of thousands of Hz, where as, the real part does not show such behavior.

Multilayer Bi1.5Zn1.0Nb1.5O7/Ba0.6Sr0.4TiO3/Bi1.5Zn1.0Nb1.5O7 thin films for tunable microwave applications

Bi1.5Zn1.0Nb1.5O7/Ba0.6Sr0.4TiO3/Bi1.5Zn1.0Nb1.5O7 tunable multilayer thin film has been fabricated by pulsed laser ablation and characterized. Phase composition and microstructure of multilayer films were characterized by X-ray diffraction, scanning electron microscopy (SEM) and atomic force microscopy (AFM). The film has very smooth surface with RMS roughness of 1.5-2nm and grain size of 100-150 nm. Total film thickness has been measure to be 375 nm. The BZN thin films at 300 K, on Pt(1 1 1)/SiO2/Si substrate showed zero-field dielectric constant of 105 and dielectric loss tangent of 0.002 at frequency of 0.1 MHz. Thin films annealed at 700 degrees C shows the dielectric tunability of 18% with biasing field 500 kV/cm at 0.1 MHz. The multilayer thin film shows nonferroelectric behavior at room temperature. The good physical and electrical properties of multilayer thin films make them promising candidate for tunable microwave device applications. (C) 2010 Elsevier B.V. All rights reserved.

Effect of nanoclay content and compatibilizer on viscoelastic properties of montmorillonite/polypropylene nanocomposites

This paper deals with preparation of nanocomposites using modified nanoclay (organoclay) and polypropylene (PP), with, and without compatibilizer (m-TMI-g-PP) to study the effects of modified nanoclay and compatibilizer on viscoelastic properties. Nanocomposites were prepared in two steps; compounding of master batch of nanoclay, polypropylene and m-TMI-g-PP in a torque rheometer and blending of this master-batch with polypropylene in a twin-screw extruder in the specific proportions to yield 3-9% nanoclay by weight in the composite. Dynamic Mechanical Analysis (DMA) tests were carried out to investigate the viscoelastic behavior of virgin polypropylene and nanocomposites. The dynamic mechanical properties such as storage modulus (E'), loss modulus (E `') and damping coefficient (tand) of PP and nano-composites were investigated with and without compatibilizer in the temperature range of -40 degrees C to 140 degrees C at a step of 5 degrees C and frequency range of 5 Hz to 100 Hz at a step of 10 Hz. Storage modulus and loss modulus of the nano-composites was significantly higher than virgin polypropylene throughout the temperature range. Storage modulus of the composites increased continuously with increasing nano-content from 3% to 9%. Composites prepared with compatibilizer exhibited inferior storage modulus than the composites without compatibilizer. Surface morphology such as dispersion of nanoclay in the composites with and without compatibilizer was analyzed through Atomic Force Microscope (AFM) that explained the differences in viscoelastic behavior of composites. (C) 2011 Elsevier Ltd. All rights reserved.

Dielectric properties of DC reactive magnetron sputtered Al2O3 thin films

Alumina (Al2O3) thin films were sputter deposited over well-cleaned glass and Si < 100 > substrates by DC reactive magnetron sputtering under various oxygen gas pressures and sputtering powers. The composition of the films was analyzed by X-ray photoelectron spectroscopy and an optimal O/Al atomic ratio of 1.59 was obtained at a reactive gas pressure of 0.03 Pa and sputtering power of 70 W. X-ray diffraction results revealed that the films were amorphous until 550 degrees C. The surface morphology of the films was studied using scanning electron microscopy and the as-deposited films were found to be smooth. The topography of the as-deposited and annealed films was analyzed by atomic force microscopy and a progressive increase in the rms roughness of the films from 3.2 nm to 4.53 nm was also observed with increase in the annealing temperature. Al-Al2O3-Al thin film capacitors were then fabricated on glass substrates to study the effect of temperature and frequency on the dielectric property of the films. Temperature coefficient of capacitance. AC conductivity and activation energy were determined and the results are discussed. (C) 2011 Elsevier B.V. All rights reserved.

AFM cantilever with integrated piezoelectric thin film for micro-actuation

This work presents micro-actuation of atomic force microscopy (AFM) cantilevers using piezoelectric Zinc Oxide (ZnO) thin film. In tapping mode AFM, the cantilever is driven near its resonant frequency by an external oscillator such as piezotube or stack of piezoelectric material. Use of integrated piezoelectric thin film for AFM cantilever eliminates the problems like inaccurate tuning and unwanted vibration modes. In this work, silicon AFM cantilevers were sputter deposited with ZnO piezoelectric film along with top and bottom metallic electrodes. The self-excitation of the ZnO coated AFM cantilever was studied using Laser Doppler Vibrometer (LDV). At its resonant frequency (227.11 kHz), the cantilever displacement varies linearly with applied excitation voltage. We observed an increase in the actuation response (131nm/V) due to improved quality of ZnO films deposited at 200 degrees C.

Composition, structure and electrical properties of DC reactive magnetron sputtered Al2O3 thin films

Thin films of alumina (Al2O3) were deposited over Si < 1 0 0 > substrates at room temperature at an oxygen gas pressure of 0.03 Pa and sputtering power of 60 W using DC reactive magnetron sputtering. The composition of the as-deposited film was analyzed by X-ray photoelectron spectroscopy and the O/Al atomic ratio was found to be 1.72. The films were then annealed in vacuum to 350, 550 and 750 degrees C and X-ray diffraction results revealed that both as-deposited and post deposition annealed films were amorphous. The surface morphology and topography of the films was studied using scanning electron microscopy and atomic force microscopy, respectively. A progressive decrease in the root mean square (RMS) roughness of the films from 1.53 nm to 0.7 nm was observed with increase in the annealing temperature. Al-Al2O3-Al thin film capacitors were then fabricated on p-type Si < 1 0 0 > substrate to study the effect of temperature and frequency on the dielectric property of the films and the results are discussed.