Mechanical characterization of porous nano-thin films by use of atomic force acoustic microscopy
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Kopycinska-Müller, M.↗
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Molecular and Nanoscale Engineering of High Efficiency Excitonic Solar Cells
We combined the synthesis of new polymers and organic-inorganic hybrid materials with new experimental characterization tools to investigate bulk heterojunction (BHJ) polymer solar cells and hybrid organic-inorganic solar cells during the 2007-2010 period (phase I) of this project. We showed that the bulk morphology of polymer/fullerene blend solar cells could be controlled by using either self-assembled polymer semiconductor nanowires or diblock poly(3-alkylthiophenes) as the light-absorbing and hole transport component. We developed new characterization tools in-house, including photoinduced absorption (PIA) spectroscopy, time-resolved electrostatic force microscopy (TR-EFM) and conductive and photoconductive atomic force microscopy (c-AFM and pc-AFM), and used them to investigate charge transfer and recombination dynamics in polymer/fullerene BHJ solar cells, hybrid polymer-nanocrystal (PbSe) devices, and dye-sensitized solar cells (DSSCs); we thus showed in detail how the bulk photovoltaic properties are connected to the nanoscale structure of the BHJ polymer solar cells. We created various oxide semiconductor (ZnO, TiO 2 ) nanostructures by solution processing routes, including hierarchical aggregates and nanorods/nanotubes, and showed that the nanostructured photoanodes resulted in substantially enhanced light-harvesting and charge transport, leading to enhanced power conversion efficiency of dye-sensitized solar cells.
14 SOLAR ENERGY↗
From Modules to Atoms: Techniques and Characterization for Identifying and Understanding Device-Level Photovoltaic Degradation Mechanisms
This report documents how degraded modules are analyzed for the characterization of cell-level performance reduction. The primary degradation topics presented here are 1) potential-induced degradation, 2) defect metastability and impurity diffusion, and 3) partial-shading-induced reverse-bias breakdown. Imaging techniques, such as electroluminescence imaging, photoluminescence imaging, and lock-in thermography provide spatial information of full modules on the meter scale. Area of interest can then be imaged with higher spatial resolution by zooming in with fields of view near the mm scale. We document procedures for coring cell samples from selected regions of interest using mechanical drilling. The small samples are then of suitable size for various microscopic analyses using techniques such as scanning electron microscopy, time-of-flight secondary ion spectrometry, atomic force microscopy, electron beam induced current, transmission electron microscopy, and atom probe tomography, which can provide chemical, structural, and electrical characterization down to the atomic scale.
14 SOLAR ENERGY↗
Poly (vinylidene fluoride-trifluoroethylene)/barium titanate nanocomposite for ferroelectric nonvolatile memory devices
The effect of barium titanate (BaTiO{sub 3}) nanoparticles (particle size <100 nm) on the ferroelectric properties of poly (vinylidenefluoride-trifluoroethylene) P(VDF-TrFE) copolymer has been studied. Different concentrations of nanoparticles were added to P(VDF-TrFE) using probe sonication, and uniform thin films were made. Polarisation - Electric field (P-E) hysteresis analysis shows an increase in remnant polarization (P{sub r}) and decrease in coercive voltage (V{sub c}). Piezo-response force microscopy analysis shows the switching capability of the polymer composite. The topography and surface roughness was studied using atomic force microscopy. It has been observed that this nanocomposite can be used for the fabrication of non-volatile ferroelectric memory devices.
77 NANOSCIENCE AND NANOTECHNOLOGY↗
Zinc oxide based diluted magnetic semiconductor nanoparticles: Synthesis by laser ablation in liquids, microstructural and optical properties
Nanoparticles of ZnO and ZnO doped with transition metals (Mn, Co) were synthesized by laser ablation in liquid medium. Scanning electron microscopy (SEM) showed formation of nanostructures with different shapes. Atomic force microscopy (AFM) gives information about surface morphology of the formed nanostructures. Absorption edge of ZnO, ZnO:Mn and ZnO:Co colloidal nanoparticles exhibits blue shift due to confinement effect. In photoluminescence spectra three peaks are attributed to the band-edge transitions and defect states. The Faraday rotation in ZnO:Mn nanoparticles gives evidence for paramagnetic behavior at room temperature.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
An (ultra) high-vacuum compatible sputter source for oxide thin film growth
A miniaturised CF-38 mountable sputter source for oxide and metal thin film preparation with enhanced high-vacuum and ultra-high-vacuum compatibility is described. The all home-built sputtering deposition device allows a high flexibility also in oxidic sputter materials, suitable deposition rates for preparation of films in the nm- and the sub-monolayer regime and excellent reliability and enhanced cleanliness for usage in UHV chambers. For a number of technologically important – yet hardly volatile – materials, the described source represents a significant improvement over thermal deposition techniques like electron-beam- or thermal evaporation, as especially the latter are no adequate tool to prepare atomically clean layers of refractory oxide materials. Furthermore, it is superior to commercially available magnetron sputter devices, especially for applications, where highly reproducible sub-monolayer thin film preparation under very clean UHV conditions is required (e.g., for studying phase boundary effects in catalysis). The device in turn offers the usage of a wide selection of evaporation materials and special target preparation procedures also allow the usage of pressed oxide powder targets. To prove the performance of the sputter-source, test preparations with technologically relevant oxide components, comprising ZrO{sub 2} and yttrium-stabilized ZrO{sub 2}, have been carried out. A wide range of characterization methods (electron microscopy, X-ray photoelectron spectroscopy, low-energy ion scattering, atomic force microscopy, and catalytic testing) were applied to demonstrate the properties of the sputter-deposited thin film systems.
36 MATERIALS SCIENCE↗
Fast time-resolved electrostatic force microscopy: Achieving sub-cycle time resolution
The ability to measure microsecond- and nanosecond-scale local dynamics below the diffraction limit with widely available atomic force microscopy hardware would enable new scientific studies in fields ranging from biology to semiconductor physics. However, commercially available scanning-probe instruments typically offer the ability to measure dynamics only on time scales of milliseconds to seconds. Here, we describe in detail the implementation of fast time-resolved electrostatic force microscopy using an oscillating cantilever as a means to measure fast local dynamics following a perturbation to a sample. We show how the phase of the oscillating cantilever relative to the perturbation event is critical to achieving reliable sub-cycle time resolution. We explore how noise affects the achievable time resolution and present empirical guidelines for reducing noise and optimizing experimental parameters. Specifically, we show that reducing the noise on the cantilever by using photothermal excitation instead of piezoacoustic excitation further improves time resolution. We demonstrate the discrimination of signal rise times with time constants as fast as 10 ns, and simultaneous data acquisition and analysis for dramatically improved image acquisition times.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
Epitaxial growth and properties of La{sub 0.7}Sr{sub 0.3}MnO{sub 3} thin films with micrometer wide atomic terraces
La{sub 0.7}Sr{sub 0.3}MnO{sub 3} (LSMO) films with extraordinarily wide atomic terraces are epitaxially grown on SrTiO{sub 3} (100) substrates by pulsed laser deposition. Atomic force microscopy measurements on the LSMO films show that the atomic step is ∼4 Å and the atomic terrace width is more than 2 μm. For a 20 monolayers (MLs) LSMO film, the magnetization is determined to be 255 ± 15 emu/cm{sup 3} at room temperature, corresponding to 1.70 ± 0.11 μ{sub B} per Mn atom. As the thickness of LSMO increases from 8 MLs to 20 MLs, the critical thickness for the temperature dependent insulator-to-metal behavior transition is shown to be 9 MLs. Furthermore, post-annealing in oxygen environment improves the electron transport and magnetic properties of the LSMO films.
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
Physical properties of RF magnetron sputtered GaN/n-Si thin film: impacts of RF power
GaN thin film was successfully produced on n-Si(100) substrate by RF magnetron sputter under different RF power. Experimental measurement techniques such as UV/Vis spectroscopy, field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), atomic force microscopy (AFM), and Micro-Raman Spectroscopy were used to research effects of Radio Frequency power on physical properties of produced thin film. It has been found that produced thin film was polycrystalline structure with (100) and (110) planes of hexagonal GaN from X-ray diffraction measurement result. It also proved that increasing RF power gives rise to deterioration in crystal quality of GaN thin film. Reason of this deterioration was discussed. It has been achieved that increasing RF power has resulted in decreasing optical band gap energy of GaN thin film. Reasons for these changes in optical band gap energy were explained. It was seen that some thin films were grown as layer-plus-island mode (Stranski–Krastanov growth mode) and others were grown as layer-by-layer growth mode (Frank van der Merwe mode) from AFM analysis. It has been found that increasing RF power has resulted in improvement of surface morphology of thin film from field emission scanning electron microscopy analysis. However, reaching RF power to 125 W leads to start to deteriorate of surface of GaN thin film. The reasons for this have been discussed. E{sub 1}(TO) transverse optical phonon mode of hexagonal GaN with different intensity was detected from Micro-Raman Spectroscopy measurement. The reasons for this difference have been discussed. It was concluded that RF power has played a significant role in growing high quality GaN thin film. Morphological, structural, and optical properties of GaN thin film were enhanced by controlling RF power, making them a potential candidate for LED, solar cell, diode application.
77 NANOSCIENCE AND NANOTECHNOLOGY↗
Polarization Control via He-Ion Beam Induced Nanofabrication in Layered Ferroelectric Semiconductors
Rapid advanced in nanoscience rely on continuous improvements of matter manipulation at near atomic scales. Currently, well characterized, robust, resist-based lithography carries the brunt of the nanofabrication process. However, use of local electron, ion and physical probe methods is also expanding, driven largely by their ability to fabricate without the multi-step preparation processes that can result in contamination from resists and solvents. Furthermore, probe based methods extend beyond nanofabrication to nanomanipulation and imaging, vital ingredients to rapid transition to prototyping and testing of layered 2D heterostructured devices. In this work we demonstrate that helium ion interaction, in a Helium Ion Microscope (HIM), with the surface of bulk copper indium thiophosphate CuM III P 2 X 6 (M = Cr, In; X= S, Se), (CITP) results in the control of ferroelectric domains, and growth of cylindrical nanostructures with enhanced conductivity; with material volumes scaling with the dosage of the beam. The nanostructures are oxygen rich, sulfur poor, and with the copper concentration virtually unchanged as confirmed by Energy Dispersive X-ray (EDX). Scanning Electron Microscopy (SEM) imaging contrast as well as Scanning Microwave Microscopy (SMM) measurements suggest enhanced conductivity in the formed particle, whereas Atomic Force Microscopy (AFM) measurements indicate that the produced structures have lower dissipation and a lower Young s modulus.
2D crystals↗
GeSn-on-insulator substrate formed by direct wafer bonding
GeSn-on-insulator (GeSnOI) on Silicon (Si) substrate was realized using direct wafer bonding technique. This process involves the growth of Ge{sub 1-x}Sn{sub x} layer on a first Si (001) substrate (donor wafer) followed by the deposition of SiO{sub 2} on Ge{sub 1-x}Sn{sub x}, the bonding of the donor wafer to a second Si (001) substrate (handle wafer), and removal of the Si donor wafer. The GeSnOI material quality is investigated using high-resolution transmission electron microscopy, high-resolution X-ray diffraction (HRXRD), atomic-force microscopy, Raman spectroscopy, and spectroscopic ellipsometry. The Ge{sub 1-x}Sn{sub x} layer on GeSnOI substrate has a surface roughness of 1.90 nm, which is higher than that of the original Ge{sub 1-x}Sn{sub x} epilayer before transfer (surface roughness is 0.528 nm). The compressive strain of the Ge{sub 1-x}Sn{sub x} film in the GeSnOI is as low as 0.10% as confirmed using HRXRD and Raman spectroscopy.
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
Effect of the Laser Scan Rate on the Microstructure, Magnetic Properties, and Microhardness of Selective Laser-Melted FeSiB
FeSiB alloys have been fabricated by selective laser melting (SLM) using a laser scan rate of 0.1–1.5 m/s, laser power of 90 W, scan line spacing of 40 μ m, and layer thickness of 50 μ m. X-ray diffraction, scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy, atomic force microscopy, profilometer, microdurometer, and vibrating sample magnetometer have been used to investigate the structural, microstructural, roughness, microhardness, and magnetic property changes during the laser melting process. The produced samples exhibit a nanocomposite structure consisting of nanocrystalline α-Fe{sub 0.95}Si{sub 0.05} and Fe{sub 2}B phases embedded into an amorphous ε-FeSi-type matrix. The selective laser-melted samples show high density, low surface roughness, higher microhardness values (1654–2273 Hv), and soft magnetic properties (M{sub s} = 188.6–199 emu/g and H{sub c} = 43.8–73 Oe).
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
Surface Modification of Rock-Forming Minerals of Diamond-Bearing Kimberlites under Interaction with Wastewater and Electrochemically Treated Water
The structural and chemical surface transformation of basic kimberlite-forming minerals (calcite, olivine, serpentine) under the contact with natural and waste mineralized water and products of electrochemical treatment of the water are studied using X-ray photoelectronic spectroscopy, scanning electron microscopy and X-ray spectral micro-analysis, and atomic force microscopy. It is found that contact with kimberlite extract and recycling water induces chemical modification of calcite surface, which consists in adsorption of hydrocarbon impurities, and chlorine- and silica-bearing compounds, majority of which are removed during interaction with the product of electrochemical treatment of recycling water. The change in the structural and chemical surface properties of rock-forming silicates, aside from adsorption–desorption of organic compound, is also connected with the distortion of nano-size layer structure after leaching of Mg, Fe and Si, and with the carbonatization of the surface.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Polarization controlled deep sub-wavelength periodic features written by femtosecond laser on nanodiamond thin film surface
Deep sub-wavelength (Λ/λ = ∼0.22) periodic features are induced uniformly on a nanodiamond (ND) thin film surface using femtosecond (fs) laser irradiation (pulse duration = ∼110 fs and central wavelength of ∼800 nm). The topography of the surface features is controlled by the laser polarization. Orientation of features is perpendicular to laser polarization. Periodicity (spatial periodicity of < λ/4) of the surface features is less than the laser wavelength. This work gives an experimental proof of polarization controlled surface plasmon-fs laser coupling mechanism prompting the interaction between fs laser and solid matter (here ND thin film) which in turn is resulting in the periodic surface features. Scanning electron microscopy in conjunction with micro Raman scattering, X-ray diffraction, and atomic force microscopy are carried out to extract surface morphology and phase information of the laser irradiated regions. This work demonstrates an easy and efficient surface fabrication technique.
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
Imaging of Unstained DNA Origami Triangles with Electron Microscopy
Imaging of scaffolded DNA and DNA origami nanostructures has been dominated by atomic force microscopy of samples immobilized on bulk substrates. Less commonly used are electron microscopy techniques, typically carried out after negative staining of DNA structures or by using cryo-transmission electron microscopy (TEM). In this work, direct imaging of unstained DNA origami on common electron-transparent substrates with utilizing high angular annular dark field scanning transmission electron microscopy (HAADF-STEM) is reported. This approach establishes a method for depositing and imaging intact DNA triangles with mass-thickness contrast sufficient to measure the scaffold-to-scaffold distances and the length of the triangle's seam. The signal-to-noise ratio (SNR) of the DNA supported on amorphous carbon as a function of the carbon thickness is measured on three types of commercially available TEM grids. This allows for edge detection of ≈1 nm height DNA triangles on carbon substrates as thick as ≈25 nm. Observations on the effect on SNR with the imaging modes are discussed. The effect of cation concentration used for pretreating the grid on the image resolution is also explored. Finally, this work presents proof-of-concept results demonstrating that electron microscopy can be used to resolve key elements of the DNA origami triangle without the use of staining protocols.
36 MATERIALS SCIENCE↗
p{sup +}-doping analysis of laser fired contacts for silicon solar cells by Kelvin probe force microscopy
Local rear contacts for silicon passivated emitter and rear contact solar cells can be established by point-wise treating an Al layer with laser radiation and thereby establishing an electrical contact between Al and Si bulk through the dielectric passivation layer. In this laser fired contacts (LFC) process, Al can establish a few μm thick p{sup +}-doped Si region below the metal/Si interface and forms in this way a local back surface field which reduces carrier recombination at the contacts. In this work, the applicability of Kelvin probe force microscopy (KPFM) to the investigation of LFCs considering the p{sup +}-doping distribution is demonstrated. The method is based on atomic force microscopy and enables the evaluation of the lateral 2D Fermi-level characteristics at sub-micrometer resolution. The distribution of the electrical potential and therefore the local hole concentration in and around the laser fired region can be measured. KPFM is performed on mechanically polished cross-sections of p{sup +}-doped Si regions formed by the LFC process. The sample preparation is of great importance because the KPFM signal is very surface sensitive. Furthermore, the measurement is responsive to sample illumination and the height of the applied voltage between tip and sample. With other measurement techniques like micro-Raman spectroscopy, electrochemical capacitance-voltage, and energy dispersive X-ray analysis, a high local hole concentration in the range of 10{sup 19 }cm{sup −3} is demonstrated in the laser fired region. This provides, in combination with the high spatial resolution of the doping distribution measured by KPFM, a promising approach for microscopic understanding and further optimization of the LFC process.
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
Comparative studies of optical and elastic properties of ZrO{sub 2} thin films prepared under normal and oblique incidence deposition geometries
Oblique angle deposited optical thin films have attracted recent researcher’s interest because of their attractive optical, micro-structural, mechanical properties and more importantly because of their great potential in achieving tunability in refractive index. These properties in turn make it important in case of designing different optical devices. In the present work, ZrO{sub 2} thin films have been deposited on fused silica substrate by electron beam evaporation technique in normal as well as oblique angle deposition configurations. Optical properties, especially refractive index of the films have been estimated by fitting the measured transmission spectra with suitable theoretical dispersion models. Atomic force microscopy has been employed to characterize morphological properties of samples. The elastic properties of both the films are estimated by Atomic Force Acoustic Microscopy, a new and highly sensitive technique for thin films.
36 MATERIALS SCIENCE↗
Prediction of the stability and electronic properties of carbon nanotori synthesized by a high-voltage pulsed discharge in ethanol vapor
An experimental technique for increasing the yield of carbon-nanotube nanotori using the modified arc synthesis method is proposed. New physical knowledge on the systematic features of the interrelation between the properties of nanotori and atomic-network topology are theoretically established for the first time. The experiments are performed based on new technology for synthesizing nanotori on nickel-catalyst particles by a high-voltage pulsed discharge in ethanol vapor and using atomic-force microscopy. Stability is predicted using an original procedure for calculating local atomic stresses. Simulation shows that the zigzag chirality corresponds to the most stable topology of nanotori. Using the tight binding method, it is shown that, depending on the chirality type, nanotori are divided into two classes, i.e., those with metal and semiconductor conductivity.
36 MATERIALS SCIENCE↗