The inverse problem in magnetic force microscopy--inferring sample magnetization from MFM images.

Nanomagnetic structures have the potential to surpass silicon's scaling limitations both as elements in hybrid CMOS logic and as novel computational elements. Magnetic force microscopy (MFM) offers a convenient characterization technique for use in the design of such nanomagnetic structures. MFM measures the magnetic field and not the sample's magnetization. As such the question of the uniqueness of the relationship between an external magnetic field and a magnetization distribution is a relevant one. To study this problem we present a simple algorithm which searches for magnetization distributions consistent with an external magnetic field and solutions to the micromagnetic equations' qualitative features. The algorithm is not computationally intensive and is found to be effective for our test cases. On the basis of our results we propose a systematic approach for interpreting MFM measurements.

Electrostatic force microscopy and potentiometry of realistic nanostructured systems

We investigate the dependency of electrostatic interaction forces on applied potentials in electrostatic force microscopy (EFM) as well as in related local potentiometry techniques such as Kelvin probe microscopy (KPM). The approximated expression of electrostatic interaction between two conductors, usually employed in EFM and KPM, may loose its validity when probe-sample distance is not very small, as often realized when realistic nanostructured systems with complex topography are investigated. In such conditions, electrostatic interaction does not depend solely on the potential difference between probe and sample, but instead it may depend on the bias applied to each conductor. For instance, electrostatic force can change from repulsive to attractive for certain ranges of applied potentials and probe-sample distances, and this fact cannot be accounted for by approximated models. We propose a general capacitance model, even applicable to more than two conductors, considering values of potentials applied to each of the conductors to determine the resulting forces and force gradients, being able to account for the above phenomenon as well as to describe interactions at larger distances. Results from numerical simulations and experiments on metal stripe electrodes and semiconductor nanowires supporting such scenario in typical regimes of EFM investigations are presented, evidencing the importance of a more rigorous modeling for EFM data interpretation. Furthermore, physical meaning of Kelvin potential as used in KPM applications can also be clarified by means of the reported formalism. © 2009 American Institute of Physics.

Development of a nanoporous and multilayer drug-delivery platform for medical implants.

Biodegradable polymers can be applied to a variety of implants for controlled and local drug delivery. The aim of this study is to develop a biodegradable and nanoporous polymeric platform for a wide spectrum of drug-eluting implants with special focus on stent-coating applications. It was synthesized by poly(DL-lactide-co-glycolide) (PLGA 65:35, PLGA 75:25) and polycaprolactone (PCL) in a multilayer configuration by means of a spin-coating technique. The antiplatelet drug dipyridamole was loaded into the surface nanopores of the platform. Surface characterization was made by atomic force microscopy (AFM) and spectroscopic ellipsometry (SE). Platelet adhesion and drug-release kinetic studies were then carried out. The study revealed that the multilayer films are highly nanoporous, whereas the single layers of PLGA are atomically smooth and spherulites are formed in PCL. Their nanoporosity (pore diameter, depth, density, surface roughness) can be tailored by tuning the growth parameters (eg, spinning speed, polymer concentration), essential for drug-delivery performance. The origin of pore formation may be attributed to the phase separation of polymer blends via the spinodal decomposition mechanism. SE studies revealed the structural characteristics, film thickness, and optical properties even of the single layers in the triple-layer construct, providing substantial information for drug loading and complement AFM findings. Platelet adhesion studies showed that the dipyridamole-loaded coatings inhibit platelet aggregation that is a prerequisite for clotting. Finally, the films exhibited sustained release profiles of dipyridamole over 70 days. These results indicate that the current multilayer phase therapeutic approach constitutes an effective drug-delivery platform for drug-eluting implants and especially for cardiovascular stent applications.

Effects of buffer layer properties and annealing process on bulk heterojunction morphology and organic solar cell performance

The performance of polymer-fullerene bulk heterojunction (BHJ) solar cells is strongly dependent on the vertical distribution of the donor and acceptor regions within the BHJ layer. In this work, we investigate in detail the effect of the hole transport layer (HTL) physical properties and the thermal annealing on the BHJ morphology and the solar cell performance. For this purpose, we have prepared solar cells with four distinct formulations of poly(3,4- ethylenedioxythiophene) poly(styrenesulfonate) (PEDOT:PSS) buffer layers. The samples were subjected to thermal annealing, applied either before (pre-annealing) or after (post-annealing) the cathode metal deposition. The effect of the HTL and the annealing process on the BHJ ingredient distribution - namely, poly(3-hexylthiophene) (P3HT) and [6,6]-phenyl C61 butyric acid methyl ester (PCBM) - has been studied by spectroscopic ellipsometry and atomic force microscopy. The results revealed P3HT segregation at the top region of the films, which had a detrimental effect on all pre-annealed devices, whereas PCBM was found to accumulate at the bottom interface. This demixing process depends on the PEDOT:PSS surface energy; the more hydrophilic the surface the more profound is the vertical phase separation within the BHJ. At the same time those samples suffer from high recombination losses as evident from the analysis of the J-V measurements obtained in the dark. Our results underline the significant effect of the HTL-active and active-ETL (electron transport layer) interfacial composition that should be taken into account during the optimization of all polymer-fullerene solar cells. © 2012 The Royal Society of Chemistry.

Thermal annealing effect on the nanomechanical properties and structure of P3HT:PCBM thin films

Nanostructured polymer-fullerene thin films are among the most prominent materials for application in high efficient polymer solar cells. Specifically, poly(3-hexylthiophene) (P3HT) and fullerene derivatives (PCBM) blends are used as the donor/acceptor materials forming a bulk heterojunction. Although P3HT:PCBM properties have been extensively studied, less light has been set on its nanomechanical properties, which affect the device service life. In this work Atomic Force Acoustic Microscopy (AFAM), Atomic Force Spectroscopy and Nanoindentation were used to study the effect of the fullerene presence and the annealing on the P3HT:PCBM nanomechanical behavior. The P3HT:PCBM thin films were prepared by spin coating on glass substrates and then annealed at 100 °C and 145 °C for 30 min. Large phase separation was identified by optical and Atomic Force Microscopy (AFM) for the annealed samples. Needle-like PCBM crystals were formed and an increase of the polymer crystallinity degree with the increase of the annealing temperature was confirmed by X-ray diffraction. AFAM characterization revealed the presence of aggregates close to stiff PCBM crystals, possibly consisting of amorphous P3HT material. AFM force-distance curves showed a continuous change in stiffness in the vicinity of the PCBM crystals, due to the PCBM depletion near its crystals, and the AFM indentation provided qualitative results about the changes in P3HT nanomechanical response after annealing. © 2011 Elsevier B.V. All rights reserved.

Efficiency measurement of GaN-based quantum well and light-emitting diode structures grown on silicon substrates

The optical efficiency of GaN-based multiple quantum well (MQW) and light emitting diode (LED) structures grown on Si(111) substrates by metal-organic vapor phase epitaxy was measured and compared with equivalent structures on sapphire. The crystalline quality of the LED structures was comprehensively characterized using x-ray diffraction, atomic force microscopy, and plan-view transmission electron microscopy. A room temperature photoluminescence (PL) internal quantum efficiency (IQE) as high as 58% has been achieved in an InGaN/GaN MQW on Si, emitting at 460 nm. This is the highest reported PL-IQE of a c-plane GaN-based MQW on Si, and the radiative efficiency of this sample compares well with similar structures grown on sapphire. Processed LED devices on Si also show good electroluminescence (EL) performance, including a forward bias voltage of ∼3.5 V at 20 mA and a light output power of 1 mW at 45 mA from a 500 ×500 μm2 planar device without the use of any additional techniques to enhance the output coupling. The extraction efficiency of the LED devices was calculated, and the EL-IQE was then estimated to have a maximum value of 33% at a current density of 4 A cm-2, dropping to 30% at a current density of 40 A cm-2 for a planar LED device on Si emitting at 455 nm. The EL-IQE was clearly observed to increase as the structural quality of the material increased for devices on both sapphire and Si substrates. © 2011 American Institute of Physics.

ZnO film based surface acoustic wave micro-pump

In this study, a micro-pump unit based on surface acoustic wave (SAW) on piezoelectric ZnO film is designed and fabricated as a micro-fluidic device. It employs a mechanical wave, which is generated electrically using an aluminum interdigital transducer (IDT), and propagates on the surface of the ZnO film. The ZnO film was used in this study because it has a high electromechanical coefficient and an excellent bonding with various substrate materials, in particular silicon. The sputtering parameters for ZnO film deposition have been optimized, and the ZnO films with different thickness from 1 micron to 5.5 microns were prepared. The film properties have been characterized using different methods, such as scanning electron microscopy, X-ray diffraction and atomic force microscopy. Aluminum IDT with a finger width and spacing of 8 microns was patterned on the ZnO film using a lift-off process. The frequency generated was measured using a network analyzer, and it varies from 130 MHz to 180 MHz as a function of film thickness. A signal generator was used to generate the frequency with a power amplifier to amplify the signal, which was then applied to aluminum IDT to generate the surface acoustic wave. If a liquid droplet exists on the surface carrying the acoustic wave, the energy and the momentum of the SAW will be coupled into the fluid, causing the liquid to vibrate and move on film surface. The strength of this movement is determined by the applied voltage and frequency. The volume of the liquid drop loaded on the SAW device in this study is of several hundreds of nanoliters. The movement of the liquid inside the droplet and also on the ZnO film surface can be demonstrated. The performance of ZnO SAW device was characterized as a function of film thickness. © 2007 IOP Publishing Ltd.

The contact of rough surfaces carrying pressure sensitive boundary layers

When two rough surfaces are loaded together it is well known that the area of true contact is very much smaller then the geometric area and that, consequently, local contact pressures are very much greater than the nominal value. If the asperities on each surface can be thought of as possessing smooth summits and each of the solids is elastically isotropic then the pressure distribution will consist of a series of small, but severe, Hertzian patches. However, if one of both of the surfaces in question is protected by a boundary layer then both the number and dimensions of these patches, and the form of the pressure distribution within them, will be modified. Recent experimental evidence from studies using both Atomic Force Microscopy and micro-tribometry suggests that boundary films produced by the action of commercial anti-wear additives, such as ZDTP, exhibit mechanical properties, which are affected by local values of pressure. These changes bring about further modifications to local conditions. These effects have been explored in a numerical model of rough surface contact and the implications for the mechanisms of surface distress and wear are discussed. © 2000 Elsevier Science B.V. All rights reserved.

Materials science: The ultrasmoothness of diamond-like carbon surfaces

The ultrasmoothness of diamond-like carbon coatings is explained by an atomistic/continuum multiscale model. At the atomic scale, carbon ion impacts induce downhill currents in the top layer of a growing film. At the continuum scale, these currents cause a rapid smoothing of initially rough substrates by erosion of hills into neighboring hollows. The predicted surface evolution is in excellent agreement with atomic force microscopy measurements. This mechanism is general, as shown by similar simulations for amorphous silicon. It explains the recently reported smoothing of multilayers and amorphous transition metal oxide films and underlines the general importance of impact-induced downhill currents for ion deposition, polishing, and nanopattering.

Increasing the design strength of glass – fractography and stress testing

Brittleness is the unintended, but inevitable consequence of producing a transparent ceramic for architectural applications such as the soda-lime glass. Its tensile strength is particularly sensitive to surface imperfections, such as that from natural weathering and malicious damage. Although a significant amount of testing of new glass has been carried out, there has been surprisingly little testing on weathered glass. Due to the variable nature of the causes of surface damage, the lack of data on weathered glass leads to a considerable degree of uncertainty in the long-term strength of exposed glass. This paper presents the results of recent tests on weathered annealed glass which has been exposed to natural weathering for more than 20 years. The tests include experimental investigations using the co-axial ring setup as well as optical and atomic force microscopy of the glass surfaces. The experimental data from these tests is subsequently used to extend existing fracture mechanics-based models to predict the strength of weathered glass. It is shown that using an automated approach based directly on finite element analysis results can give an increase in effective design strength in the order of 70 to 100% when compared to maximum stress methods. It is also shown that by combining microscopy and strength test results, it is possible to quantitatively characterise the damage on glass surfaces.

Ferroelectric-carbon nanotube memory devices

One-dimensional ferroelectric nanostructures, carbon nanotubes (CNT) and CNTinorganic oxides have recently been studied due to their potential applications for microelectronics. Here, we report coating of a registered array of aligned multi-wall carbon nanotubes (MWCNT) grown on silicon substrates by functional ferroelectric Pb(Zr,Ti)O 3 (PZT) which produces structures suitable for commercial prototype memories. Microstructural analysis reveals the crystalline nature of PZT with small nanocrystals aligned in different directions. First-order Raman modes of MWCNT and PZT/MWCNT/n-Si show the high structural quality of CNT before and after PZT deposition at elevated temperature. PZT exists mostly in the monoclinic Cc/Cm phase, which is the origin of the high piezoelectric response in the system. Lowloss square piezoelectric hysteresis obtained for the 3D bottom-up structure confirms the switchability of the device. Currentvoltage mapping of the device by conducting atomic force microscopy (c-AFM) indicates very low transient current. Fabrication and functional properties of these hybrid ferroelectriccarbon nanotubes is the first step towards miniaturization for future nanotechnology sensors, actuators, transducers and memory devices. © 2012 IOP Publishing Ltd.

Controllable chemical vapor deposition of large area uniform nanocrystalline graphene directly on silicon dioxide

Metal-catalyst-free chemical vapor deposition (CVD) of large area uniform nanocrystalline graphene on oxidized silicon substrates is demonstrated. The material grows slowly, allowing for thickness control down to monolayer graphene. The as-grown thin films are continuous with no observable pinholes, and are smooth and uniform across whole wafers, as inspected by optical-, scanning electron-, and atomic force microscopy. The sp 2 hybridized carbon structure is confirmed by Raman spectroscopy. Room temperature electrical measurements show ohmic behavior (sheet resistance similar to exfoliated graphene) and up to 13 of electric-field effect. The Hall mobility is ∼40 cm 2/Vs, which is an order of magnitude higher than previously reported values for nanocrystalline graphene. Transmission electron microscopy, Raman spectroscopy, and transport measurements indicate a graphene crystalline domain size ∼10 nm. The absence of transfer to another substrate allows avoidance of wrinkles, holes, and etching residues which are usually detrimental to device performance. This work provides a broader perspective of graphene CVD and shows a viable route toward applications involving transparent electrodes. © 2012 American Institute of Physics.

Properties of trench defects in InGaN/GaN quantum well structures

The structural and optical properties of trench defects, which are poorly understood yet commonly occurring defects observed on the surfaces of InGaN multiple quantum wells (MQW), are reported. These defects comprise near-circular trenches which enclose areas of MQW which give rise to a red shift in peak photoluminescence emission and a change in cathodoluminescence intensity with respect to the surrounding material. Atomic force microscopy shows that the height of trench-enclosed areas differs from that of the surrounding quantum well structure, and that trenches are unrelated to the commonly observed V-defects in InGaN films, despite being occasionally intersected by them. Cross-sectional electron microscopy analysis of trenches with raised centres suggests that the red shift in the observed cathodoluminescence peak emission may be due to the quantum wells being thicker in the trench-enclosed regions than in the surrounding quantum well area. The mechanism of trench formation and its implication for the control of the emission properties of light-emitting diodes is discussed. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Correlations between the morphology and emission properties of trench defects in InGaN/GaN quantum wells

Atomic force microscopy (AFM) and scanning electron microscopy (SEM) with cathodoluminescence (CL) were performed on exactly the same defects in a blue-emitting InGaN/GaN multiple quantum well (QW) sample enabling the direct correlation of the morphology of an individual defect with its emission properties. The defects in question are observed in AFM and SEM as a trench partially or fully enclosing a region of the QW having altered emission properties. Their sub-surface structure has previously been shown to consist of a basal plane stacking fault (BSF) in the plane of the QW stack, and a stacking mismatch boundary (SMB) which opens up into a trench at the sample surface. In CL, the material enclosed by the trench may emit more or less intensely than the surrounding material, but always exhibits a redshift relative to the surrounding material. A strong correlation exists between the width of the trench and both the redshift and the intensity ratio, with the widest trenches surrounding regions which exhibit the brightest and most redshifted emission. Based on studies of the evolution of the trench width with the number of QWs from four additional MQW samples, we conclude that in order for a trench defect to emit intense, strongly redshifted light, the BSF must be formed in the early stages of the growth of the QW stack. The data suggest that the SMB may act as a non-radiative recombination center. © 2013 American Institute of Physics.

Self-assembled multilayer graphene oxide membrane and carbon nanotubes synthesized using a rare form of natural graphite

The fabrication of flexible multilayer graphene oxide (GO) membrane and carbon nanotubes (CNTs) using a rare form of high-purity natural graphite, vein graphite, is reported for the first time. Graphite oxide is synthesized using vein graphite following Hummer's method. By facilitating functionalized graphene sheets in graphite oxide to self-assemble, a multilayer GO membrane is fabricated. Electric arc discharge is used to synthesis CNTs from vein graphite. Both multilayer GO membrane and CNTs are investigated using microscopy and spectroscopy experiments, i.e., scanning electron microscopy (SEM), atomic force microscopy (AFM), high-resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), core level photoelectron spectroscopy, and C K-edge X-ray absorption spectroscopy (NEXAFS), to characterize their structural and topographical properties. Characterization of vein graphite using different techniques reveals that it has a large number of crystallites, hence the large number of graphene sheets per crystallite, preferentially oriented along the (002) plane. NEXAFS and core level spectra confirm that vein graphite is highly crystalline and pure. Fourier transform infrared (FT-IR) and C 1s core level spectra show that oxygen functionalities (-C-OH, -CO,-C-O-C-) are introduced into the basal plane of graphite following chemical oxidation. Carbon nanotubes are produced from vein graphite through arc discharge without the use of any catalyst. HRTEM confirm that multiwalled carbon nanotube (MWNTs) are produced with the presence of some structure in the central pipe. A small percentage of single-walled nanotubes (SWNTs) are also produced simultaneously with MWNTs. Spectroscopic and microscopic data are further discussed here with a view to using vein graphite as the source material for the synthesis of carbon nanomaterials. © 2013 American Chemical Society.