Materials For Micro Research Articles

Si/Ge core–shell nanoarrays as the anode material for 3D lithium ion batteries

The rapid development of small scale electronic devices, such as M/NEMS devices, smart dust, micro or nano bio-sensors and so on, is leading to the urgent need for micro or nano power sources with the possibility for integration. In this work, 3D Si/Ge composite nanorod (NR) arrays were fabricated on wafer-scale Si substrates as anode materials in micro or nano Li ion batteries (LIBs) by a low cost, simple and Si-compatible process. Significantly improved capacities and cycling performances were accomplished in the optimized 3D Si/Ge composite NR array electrode by successfully addressing the volume expansion and conductivity issues. Further theoretical calculations gain more insights into the origins of the improved electrochemical properties by considering the adsorption and diffusion energies of Li ion in Si and Si/Ge unit cells. This study technically and fundamentally provides a perspective idea for practical applications of wafer-scale Si substrates in LIBs with the aim of supplying integrated power for micro or nano scale electronic devices.

Towards Quantitative Characterisation of the Small Force Transducer Used in Nanoindentation Instruments

Quantitative characterization of the mechanical properties of materials in micro-/nano-scale using depth-sensing indentation technique demands high performance of nanoindentation instruments in use. In this paper, the efforts to calibrate the capacitive force transducer of a commercial nanoindentation instrument are presented, where the quasi-static characteristic of the force transducer has been calibrated by a precise compensation balance with a resolution of ~1 nN. To investigate the dynamic response of the transducer, an electrostatic MEMS (Micro-Electro-Mechanical System) based on nano-force transfer standard with nano-Newton (10-9 Newton) resolution and a bandwidth up to 6 kHz have been employed. Preliminary experimental results indicate that 1) the force transducer under calibration has a probing force uncertainty less than 300 nN (1σ) in the calibration range of 1 mN; 2) the transient duration at contact points amounts to 10 seconds; 3) the overshoot of engagement is pre-load dependent.

Characterization of low temperature deposited atomic layer deposition TiO2 for MEMS applications

TiO2 is an interesting and promising material for micro-/nanoelectromechanical systems (MEMS/NEMS). For high performance and reliable MEMS/NEMS, optimization of the optical characteristics, mechanical stress, and especially surface smoothness of TiO2 is required. To overcome the roughness issue of the TiO2 films due to crystallization during deposition at high temperatures (above 250 °C), low temperature (80–120 °C) atomic layer deposition (ALD) is investigated. By lowering the deposition temperature, the surface roughness significantly decreases from 3.64 nm for the 300 °C deposited crystalline (anatase phase) TiO2 to 0.24 nm for the 120 °C amorphous TiO2. However, the layers deposited at low temperature present different physical behaviors comparing to the high temperature ones. The refractive index drops from 2.499 to 2.304 (at 633 nm) and the stress sharply decreases from 684 to 133 MPa. Superhydrophilic surface is obtained for the high temperature deposited TiO2 under ultraviolet illumination, while little changes are found for the low temperature TiO2. The authors demonstrate that by suitable postdeposition annealing, all the properties of the low temperature deposited films recover to that of the 300 °C deposited TiO2, while the smooth surface profile (less than 1 nm roughness) is maintained. Finally, micromachining of the low temperature ALD TiO2 by dry etching is also studied.

Warpage Measurement of a Micro Electrical Fan on Micro-Injection Molding

This study characterizes warpage of a micro-injection molded micro electrical fan using the Michelson interference method. This study conducts experiments to analyze different polymers-polypropylene (PP), polyamide (PA), acrylonitrile-butadiene styrene (ABS), ABS+ polycarbonate (PC), and polyoxymethylene (POM)-process parameters, such as mold temperature, injection temperature, injection pressure, injection time, packing time, and packing pressure, for a micro electrical fan. To obtain the optimum result (minimum warpage), this study assesses the effect (warpage) of each material on micro-injection molding. PA plastic is the very suitable material for micro electrical fan with Michelson interference analysis on micro-injection molding.

Stress Evaluation on Hetero-Epitaxial 3C-SiC Film on (100) Si Substrates

SiC is a candidate material for micro- and nano-electromechanical systems (MEMS and NEMS). In order to understand the impact that the growth rate has on the residual stress of CVD-grown 3C-SiC hetero-epitaxial films on Si substrates, growth experiments were performed and the resulting stress was evaluated. Film growth was performed using a two-step growth process with propane and silane as the C and Si precursors in hydrogen carrier gas. The film thickness was held constant at ~2.5 µm independent of the growth rate so as to allow for direct films comparison as a function of the growth rate. Supported by profilometry, Raman and micro-machined free-standing structures, this study shows that the growth rate is a fundamental parameter for low-defect and low-stress hetero-epitaxial growth process of 3C-SiC on Si substrates. Stress analysis performed by modify Stoney’s equation trough optical curvature measurement, Raman shift analysis and micro-machining of free-standing structures that shows apparent disagreement about the nature of the stress. These odds between the experimental data can be explained assuming a strong stress field located in the substrate and related to defects generated in the silicon during the growth process.

Mechanical Proprieties and Residual Stress Evaluation on Heteroepitaxial 3C-SiC/Si for MEMS Application

SiC is a candidate material for micro- and nano-electromechanical systems (MEMS and NEMS). The hetero-epitaxial growth of 3C-SiC on silicon substrates allows one to overcome the traditional limitations of SiC micro-fabrication, but the high residual stress created during the film grow limits the development of the material for these applications. In this work, in order to evaluate the amount of residual stress released from the epi-film, different micro-machined structures were developed. Through the measurement of natural resonant frequencies and Raman shift analysis, a strong relationship between the mechanical proprieties of the material (Young’s modulus) and the film crystal quality (defect density) was observed.

Development of methods of surface analysis in Russia

The present paper reviews the studies of Russian scientists devoted to the analysis of the surface of solids in 1991–2010. A special attention was paid to the determination of the chemical composition of surfaces of advanced materials and materials for micro- and nanoelectronics by means of electron, ion, and X-ray spectroscopy.

Advanced Stress Analysis by Micro-Structures Realization on High Quality Hetero-Epitaxial 3C-SiC for MEMS Application

SiC is a candidate material for micro- and nano-electromechanical systems (MEMS and NEMS). The fabrication of SiC MEMS-based sensors requires new processes able to realize microstructures on either bulk material or on the SiC surface. The hetero-epitaxial growth of 3C-SiC on silicon substrates allows one to overcome the traditional limitations of SiC micro-fabrication, but the high residual stress created during the film grow limits the development of the material for these applications. In order to evaluate the amount of residual stress released from the epi-film, different micro-machined structures were developed. Finite elements simulations of the micro-machined structures have also been carried out in order to evaluate, in detail, the stress field inside the structures and to test the analytical model used. With finite element modeling a exponential approximation of the stress relationship was studied, yielding a better fit with the experimental data. This study shows that this new approximation of the total residual stress function reduces the disagreement between experimental and simulated data.

Defect Influence on Heteroepitaxial 3C-SiC Young’s Modulus

Heteroepitaxial cubic silicon carbide (3C-SiC) is an extremely promising material for micro- and nano-electromechanical systems due to its large Young’s modulus. Unfortunately, the heteroepitaxy of 3C-SiC on Si substrate is affected by the high mismatch in the lattice parameters and the thermal expansion coefficients between the two dissimilar materials that generate a high number of defects in the material. In this work, through the measurement of natural resonant frequencies and Raman shift analysis, a strong relationship between the mechanical proprieties of the material (Young’s modulus) and the film crystal quality (defect density)

Volume confinement induced microstructural transitions and property enhancements of supramolecular soft materials

The rheological properties of supramolecular soft functional materials are determined by the networks within the materials. This research reveals for the first time that the volume confinement during the formation of supramolecular soft functional materials will exert a significant impact on the rheological properties of the materials. A class of small molecular organogels formed by the gelation of N-lauroyl-L-glutamic acid din-butylamide (GP-1) in ethylene glycol (EG) and propylene glycol (PG) solutions were adopted as model systems for this study. It follows that within a confined space, the elasticity of the gel can be enhanced more than 15 times compared with those under un-restricted conditions. According to our optical microscopy observations and rheological measurements, this drastic enhancement is caused by the structural transition from a multi-domain network system to a single network system once the average size of the fiber network of a given material reaches the lowest dimension of the system. The understanding acquired from this work will provide a novel strategy to manipulate the network structure of soft materials, and exert a direct impact on the micro-engineering of such supramolecular materials in micro and nano scales.

Probing mechanical properties of thin film and ceramic materials in micro- and nano-scale using indentation techniques

In this study, we report on the mechanical properties, failure and fracture modes in two cases of engineering materials; that is transparent silicon oxide thin films onto poly(ethylene terephthalate) (PET) membranes and glass-ceramic materials. The first system was studied by the quazi-static indentation technique at the nano-scale and the second by the static indentation technique at the micro-scale. Nanocomposite laminates of silicon oxide thin films onto PET were found to sustain higher scratch induced stresses and were effective as protective coating material for PET membranes. Glass-ceramic materials with separated crystallites of different morphologies sustained a mixed crack propagation pattern in brittle fracture mode.

Spectroscopic Studies of Polycrystalline NaAl(MoO<SUB>4</SUB>)<SUB>2</SUB>:Cr<SUP>3+</SUP> Compound as New Material for Micro- and Nano-Sized Cryogenic Fluorescence Thermometer

Spectroscopic Studies of Polycrystalline NaAl(MoO<SUB>4</SUB>)<SUB>2</SUB>:Cr<SUP>3+</SUP> Compound as New Material for Micro- and Nano-Sized Cryogenic Fluorescence Thermometer

Growth Rate Effect on 3C-SiC Film Residual Stress on (100) Si Substrates

SiC is a candidate material for micro- and nano-electromechanical systems (MEMS and NEMS). In order to understand the impact that the growth rate has on the residual stress of CVD-grown 3C-SiC hetero-epitaxial films on Si substrates, growth experiments were performed and the resulting stress was evaluated. Film growth was performed using a two-step growth process with propane and silane as the C and Si precursors in hydrogen carrier gas. The film thickness was held constant at ~2.5 µm independent of the growth rate so as to allow for direct films comparison as a function of the growth rate. Supported by profilometry, Raman and XRD analysis, this study shows that the growth rate is a fundamental parameter for low-defect and low-stress hetero-epitaxial growth process of 3C-SiC on Si substrates. XRD (rocking curve analysis) and Raman spectroscopy show that the crystal quality of the films increases with decreasing growth rate. From curvature measurements, the average residual stress within the layer using the modified Stoney’s equation was calculated. The results show that the films are under compressive stress and the calculated residual stress also increases with growth rate, from -0.78 GPa to -1.11 GPa for 3C-SiC films grown at 2.45 and 4 µm/h, respectively.

Synthesis and Field Emission Properties of Ultra-Nanocrystalline Diamond Fibers and Helices

We propose a novel template method for large scale synthesis of Ultra-Nanocrystalline Diamond (UNCD) fibres and helices with lengths of thousands of microns and diameters ranging from 0.5 to 5 microm: (i) Large quantities of submicrometer- or nanometer-diameter silica (a-SiO2) nanostructures, with lengths in the order of 2 to 4 mm, were synthesized by Vapor-Liquid-Solid (VLS) method; (ii) UNCD coating of as-synthesized a-SiO2 micro- or nanonanostructures by Microwave Plasma Chemical Vapour Deposition (MPCVD) technique in hydrogen-deficient condition. Electron Field Emission (EFE) of as-synthesized UNCD structures was observed with a threshold field of 3.4 V/microm. These micro- or nanostructures may find potential applications in high power electronics, vertical field-effect transistors in vacuum electronics, heat sinks in microelectronics and structural materials in Micro- and Nano-Electro-Mechanical Systems (MEMS/NEMS). The successful preparation of various types of UNCD structures suggests that this templating process can be used for a wide range of materials.

Colloidal Inorganic Nanocrystal Based Nanocomposites: Functional Materials for Micro and Nanofabrication

The unique size- and shape-dependent electronic properties of nanocrystals (NCs) make them extremely attractive as novel structural building blocks for constructing a new generation of innovative materials and solid-state devices. Recent advances in material chemistry has allowed the synthesis of colloidal NCs with a wide range of compositions, with a precise control on size, shape and uniformity as well as specific surface chemistry. By incorporating such nanostructures in polymers, mesoscopic materials can be achieved and their properties engineered by choosing NCs differing in size and/or composition, properly tuning the interaction between NCs and surrounding environment. In this contribution, different approaches will be presented as effective opportunities for conveying colloidal NC properties to nanocomposite materials for micro and nanofabrication. Patterning of such nanocomposites either by conventional lithographic techniques and emerging patterning tools, such as ink jet printing and nanoimprint lithography, will be illustrated, pointing out their technological impact on developing new optoelectronic and sensing devices.

Some Preliminary Metallurgical Studies on Grain Size and Density of Work Material used in Micro Turning Operation

One important process in tool based micro machining technology is CNC micro turning which has the capability to produce 3D structures on micro scale. The major drawback of micro turning process is that the machining force influences machining accuracy and the limit of machinable size and shape. Therefore, the control of reactive force during cutting is an important factor in improving machining accuracy. The properties of work material significantly affect the cutting force generated during turning process. Commercially available metal rods are inhomogeneous and hence, qualifying the right material is very crucial in micro turning. Unlike plates, the properties like grain size and density vary significantly at different locations of the round bars. Hence, it is found very important to systematically find right material for micro turning from the commercially available rods. In present study, an attempt has been made to study the grain size and density of blank material from different locations of a larger diameter shaft. The work material selected is a 32 mm diameter shaft of commercial brass, a non ferrous alloy of copper and zinc. Five samples from different radial locations are cut from this shaft. It is found that grains are coarser at centre and finer towards the periphery of the shaft. Further, local density is less at centre and high at periphery of the shaft.

Strain engineering and one-dimensional organization of metal–insulator domains in single-crystal vanadium dioxide beams

Correlated electron materials can undergo a variety of phase transitions, including superconductivity, the metal-insulator transition and colossal magnetoresistance. Moreover, multiple physical phases or domains with dimensions of nanometres to micrometres can coexist in these materials at temperatures where a pure phase is expected. Making use of the properties of correlated electron materials in device applications will require the ability to control domain structures and phase transitions in these materials. Lattice strain has been shown to cause the coexistence of metallic and insulating phases in the Mott insulator VO(2). Here, we show that we can nucleate and manipulate ordered arrays of metallic and insulating domains along single-crystal beams of VO(2) by continuously tuning the strain over a wide range of values. The Mott transition between a low-temperature insulating phase and a high-temperature metallic phase usually occurs at 341 K in VO(2), but the active control of strain allows us to reduce this transition temperature to room temperature. In addition to device applications, the ability to control the phase structure of VO(2) with strain could lead to a deeper understanding of the correlated electron materials in general.

Microstructural, mechanical and magnetic properties of shape memory alloy Ni 55Mn 23Ga 22 thin films deposited by radio-frequency magnetron sputtering

The near-stoichiometric Ni 2MnGa ferromagnetic alloys are one of the smart materials, that are of a great interest when they are deposited as a thin film by r.f. sputtering. These thin films of shape memory alloys are prospective materials for micro and nanosystem applications. However, the properties of the shape memory polycrystalline thin films depend strongly on their structure and internal stress, which develop during the sputtering process as well as during the post-deposition annealing treatment. In this study, about 1 μm Ni 55Mn 23Ga 22 thin films were deposited in the range 0,45 to 1,2 Pa of Ar pressure and P = 40 to 120 W. Their composition, crystallographic structure, internal stress and stress gradient, indentation modulus, hardness, deflection induced by magnetic field and magnetic properties were systematically studied as a function of the temperature of the silicon substrate ranging from 298 to 873 K and the vacuum annealing treatment at 873 K for 21,6 ks and 36 ks. A silicon wafer having a native amorphous thin SiO x buffer layer was used as a substrate. This substrate influences the microstructure of the films and blocks the diffusion process during the heat treatment. The crystal structure of the martensitic phase in each film was changed systematically from bct or 10 M or 14 M. In addition, the evolution of the mechanical properties such as mean stress, stress gradient, roughness, hardness and indentation modulus with the temperature (of substrate or of heat treatment) were measured and correlated to crystal structure and morphology changes. Moreover, it has been shown that it is necessary to associate a high temperature (873 K) annealing during a long time (21 ks and 36 ks) to obtain good ferromagnetic properties. Thus, for the well annealed films (36 ks at 873 K) the magnetostrain is about - 170 ppm for a magnetic field of 1 MA m - 1 applied along the beams. As a conclusion, the response of free-standing magnetic shape memory films to a magnetic field of 0,2 MA m - 1 depends strongly on the martensitic structure, internal mechanical stress (mean and gradient) and magnetic properties. The free-standing annealed film at 873 K for 36 ks points out a considerable magnetic actuation associated with bct or 10 M or 14 M martensitic structures.

Fabrication and Characterization of Graphitic Carbon Nanostructures with Controllable Size, Shape, and Position

The incorporation of carbon materials in micro- and nanoscale devices is being widely investigated due to the promise of enhanced functionality. Challenges in the positioning and addressability of carbon nanotubes provide the motivation for the development of new processes to produce nanoscale carbon materials. Here, the fabrication of conducting, nanometer-sized carbon structures using a combination of electron beam lithography (EBL) and carbonisation is reported. EBL is used to directly write predefined nanometer-sized patterns in a thin layer of negative resist in controllable locations. Careful heat treatment results in carbon nanostructures with the size, shape, and location originally defined by EBL. The pyrolysis process results in significant shrinkage of the structures in the vertical direction and minimal loss in the horizontal direction. Characterization of the carbonized material indicates a structure consisting of both amorphous and graphitized carbon with low levels of oxygen. The resistivity of the material is similar to other disordered carbon materials and the resistivity is maintained from the bulk to the nanoscale. This is demonstrated by fabricating a nanoscale structure with predictable resistance. The ability to fabricate these conductive structures with known dimensions and in predefined locations can be exploited for a number of applications. Their use as nanoband electrodes is also demonstrated.

437 マイクロカプセル潜熱蕃熱材(MEPCM)を用いた複合材料の非定常熱伝導 : 実験と数値計算との比較(蓄熱・電力貯蔵技術)

437 マイクロカプセル潜熱蕃熱材(MEPCM)を用いた複合材料の非定常熱伝導 : 実験と数値計算との比較(蓄熱・電力貯蔵技術)