Transient liquid crystal thermometry of microfabricated PCR vesselarrays

Polymerase chain reaction (PCR) using micromachined structures promises improved temperature uniformity and cycling time together with decreased reagent and sample volumes. Thermal design of these structures will benefit from measurements of the temperature distribution in the reacting liquid. We report measurements of temperature uniformity and time constant in a microfabricated 18-vessel array using encapsulated liquid crystals suspended in the liquid. Separate sets of crystals are used to image temporal and spatial temperature variations near the processing thresholds of 55°C and 95°C with a resolution of 0.1°C. While the thermometry technique developed here is particularly useful for characterizing microfabricated PCR systems, it can also aid with the thermal design of a broad variety of microfluidic devices     

Microfabricated small metal cantilevers with silicon tip for atomicforce microscopy

Atomic force microscopy with small cantilevers is faster due to higher resonant frequencies and has a lower noise level. We report a new process to microfabricate small metal cantilevers with integrated silicon tips. This process is used to fabricate gold cantilevers that are 13-40-μm long, 5-10-μm wide, and 100-160-nm thick. The tip is first formed at the free end of a sacrificial oxide cantilever. The cantilever layer of the desired metal is then deposited on the nontip side of the sacrificial oxide cantilever. The oxide layer is removed to form the cantilevers with tips on them in a batch process. The highly stressed cantilevers are rapid thermal annealed for 60 s at 300°C to relieve the stress. The gold cantilevers have been characterized through their thermal spectra and used to image in tapping mode. The process can be used, not only for gold, but also for any metal or compound that can withstand removal of sacrificial oxide cantilevers     

Dichlorodimethylsilane as an anti-stiction monolayer for MEMS: acomparison to the octadecyltrichlorosilane self-assembled monolayer

This paper presents a quantitative comparison of the dichlorodimethylsilane (DDMS) monolayer to the octade-cyltrichlorosilane (OTS) self-assembled monolayer (SAM) with respect to the film properties and their effectiveness as anti-stiction coatings for micromechanical structures. Both coatings have been evaluated in several ways, including atomic force microscopy (AFM), contact angle analysis (CAA), work of adhesion by cantilever beam array (CBA) technique and coefficient of static friction using a sidewall testing device. While water and hexadecane contact angles are comparable, the DDMS coated microstructures exhibit higher adhesion than OTS coated ones. Furthermore, coefficient of static friction data indicate that the DDMS films are not as effective at lubrication as the OTS SAMs are, although both exhibit much improvement over chemical oxide. However, AFM data show that the samples which receive DDMS treatment accumulate fewer particles during processing than those which receive the OTS SAM treatment. The thermal stability of the DDMS film in air far exceeds the OTS SAM, as the DDMS remains very hydrophobic to temperatures upwards of 400°C     

A hermetic glass-silicon micropackage with high-density on-chipfeedthroughs for sensors and actuators

This paper describes the development of a hermetic micropackage with high-density on-chip feedthroughs for sensor and actuator applications. The packaging technique uses low-temperature (320°C) electrostatic bonding of a custom-made glass capsule (Corning 7740, 2×2×8 mm³) to fine grain polysilicon in order to form a hermetically sealed cavity. High-density on-chip multiple polysilicon feedthroughs (200 per millimeter) are used for connecting external sensors and actuators to the electronic circuitry inside the package. A high degree of planarity over feedthrough areas is obtained by using grid-shaped polysilicon feedthrough lines that are covered with phosphosilicate glass (PSG), which is subsequently reflown at 1100°C in steam for 2 h. Saline and DI water soak tests at elevated temperatures (85 and 95°C) were performed to determine the reliability of the package. Preliminary results have shown a mean time to failure (MTTF) of 284 days and 118 days at 85 and 95°C, respectively, in DI water. An Arrhenius diffusion model for moisture penetration yields an expected lifetime of 116 years at body temperature (37°C) for these packages. In vivo tests in guinea pigs and rats for periods ranging from one to two months have shown no sign of infection, inflammation, or tissue abnormality around the implanted package     

Thin film shape memory alloy microactuators

Thin film shape memory alloys (SMAs) have the potential to become a primary actuating mechanism for mechanical devices with dimensions in the micron-to-millimeter range requiring large forces over long displacements. The work output per volume of thin film SMA microactuators exceeds that of other microactuation mechanisms such as electrostatic, magnetic, thermal bimorph, piezoelectric, and thermopneumatic, and it is possible to achieve cycling frequencies on the order of 100 Hz due to the rapid heat transfer rates associated with thin film devices. In this paper, a quantitative comparison of several microactuation schemes is made, techniques for depositing and characterizing Ni-Ti-based shape memory films are evaluated, and micromachining and design issues for SMA microactuators are discussed. The substrate curvature method is used to investigate the thermo-mechanical properties of Ni-Ti-Cu SMA films, revealing recoverable stresses up to 510 MPa, transformation temperatures above 32°C, and hysteresis widths between 5 and 13°C. Fatigue data shows that for small strains, applied loads up to 350 MPa can be sustained for thousands of cycles. Two micromachined shape memory-actuated devices-a microgripper and microvalve-also are presented     

A three-dimensional shape memory alloy microelectrode with clippingstructure for insect neural recording

A microelectrode, with clipping structure for neural recording from a free-moving insect, was designed and fabricated using a shape memory alloy (SMA) thin film. The SMA thin films (titanium nickel; Ti-48 at.%Ni) are deposited by RF magnetron sputtering and patterned by HF-HNO ₃ wet etching. The transformation temperatures of the SMA thin films were measured at 54°C (A*) and 50°C (M*). The SMA microelectrode consists of a “hook” structure (720 μm×480 μm) and two “C”-shape probes (600 μm×70 μm). The electrode impedance is about 5 kΩ at 1 kHz. The desired three-dimensional (3D) shape is given to the electrode by a bonded wire. The clinging force of the electrode to the nerve is enhanced by the 3-D structures. The SMA microelectrode can clip a nerve cord tightly. The damages of the nerve by thermal actuation of the clip are not observed by physiological analysis. The neural activity from a living insect was successfully recorded with this SMA microelectrode     

Localized silicon fusion and eutectic bonding for MEMS fabricationand packaging

Silicon fusion and eutectic bonding processes based on the technique of localized heating have been successfully demonstrated. Phosphorus-doped polysilicon and gold films are applied separately in the silicon-to-glass fusion bonding and silicon-to-gold eutectic bonding experiments. These films are patterned as line-shape resistive heaters with widths of 5 or 7 μm for the purpose of heating and bonding. In the experiments, silicon-to-glass fusion bonding and silicon to gold eutectic bonding are successfully achieved at temperatures above 1000°C and 800°C, respectively, by applying 1-MPa contact pressure. Both bonding processes can achieve bonding strength comparable to the fracture toughness of bulk silicon in less than 5 min. Without using global heating furnaces, localized bonding process is conducted in the common environment of room temperature and atmospheric pressure. Although these processes are accomplished within a confined bonding region and under high temperature, the substrate temperature remains low. This new class of bonding scheme has potential applications for microelectromechanical systems fabrication and packaging that require low-temperature processing at the wafer level, excellent bonding strength, and hermetic sealing characteristics     

The development of a low-stress polysilicon process compatible withstandard device processing

When surface micromachined devices are combined with on-chip circuitry, any high-temperature processing must be avoided to minimize the effect on active device characteristics. High-temperature stress annealing cannot be applied to these structures. This work studies the effects of deposition parameters and subsequent processing on the mechanical properties of the polysilicon film in the development of a low-strain polysilicon process, without resorting to high-temperature annealing. The films are deposited as a semi-amorphous film and then annealed, in situ at 600°C for 1 h, to ensure the desired mechanical characteristics for both doped and undoped samples. This low temperature anneal changes the strain levels in undoped films from -250 to +1100 με. The best results have been obtained for an 850°C anneal for 30 min which is used to activate the dopant (both phosphorus and boron). No further stress annealing was used, and 850°C does not present problems in terms of thermal budget for the electrical devices. It is shown that these mechanical characteristics are achieved by forming the grain boundaries during subsequent low temperature annealing, and not during deposition. TEM (transmission electron microscopy) studies have been used to investigate the link between the structure and mechanical strain. This has shown that it is the formation of the grain boundary rather than the grain size which has a significant effect on strain levels, contrary to reports in the literature. Using the above-mentioned deposition process, a series of experiments have been performed to establish the flexibility in subsequent processing available to the designer. Therefore, by careful consideration of the processing, a low-temperature polysilicon process, which can be used to fabricate thin micromachined structures, has been developed     

TiO2 thin films from titanium butoxide: Synthesis, Pt addition, structural stability, microelectronic processing and gas-sensing properties

TiO₂ thin films were prepared by spin-coating of a Ti butoxide-derived sol onto oxidized silicon wafers, followed by a heat-treatment at temperatures ranging from 500 to 800 °C. The film thickness after heat-treatment at 500 °C was 50 nm. Pt addition, with a Pt:Ti nominal atomic ratio ranging from 0.01 to 0.1, was achieved by adding solutions of Pt(II) acetylacetonate to the TiO₂ sols. The thin films were investigated by X-ray diffraction, evidencing that Pt promoted the structural transformation of the starting anatase phase of TiO₂ to rutile, with a more enhanced effect with increasing the Pt concentration and/or the heat-treatment temperature. High-resolution transmission electron microscopy evidenced that, when a Pt:Ti atomic ratio of 0.05 and a heat treatment at 500 °C were used, the TiO₂ contained both anatase and rutile phases and interspersed Pt nanocrystals (2–3 nm). This result allowed attributing the structural transformation in TiO₂ to the strain created by the Pt nanocrystals—a conclusion which was further corroborated by the observation that Pd-modified films, prepared under similar conditions, were only composed of anatase TiO₂ and did not contain any Pd nanocrystals. The films heat-treated at 500 °C were able to withstand a full microelectronic processing sequence, including dry etching for gas sensors sensitive area definition, Ti/Pt contact formation, and heater processing on the backside of the sensor substrates. H₂ gas-sensing tests evidenced that the anatase TiO₂ phase was much more sensitive than the rutile one. The presence of Pt further enhanced the gas-sensing properties, lowering the optimum sensor operation temperature to about 330 °C and allowing for the detection of a minimum H₂ concentration of about 1000 ppm.     

Structural and mechanical properties of polycrystalline silicongermanium for micromachining applications

In this paper, we propose polycrystalline silicon germanium (poly SiGe) as a material suitable for MEMS applications. Films are prepared by chemical vapor deposition (CVD) at atmospheric pressure (AP) or reduced pressure (RP). The structure of the films is investigated by X-ray diffraction (XRD) and transmission electron microscopy (TEM) for different deposition and annealing conditions. The stress in the as-grown and annealed layers is measured, and the correlation between stress and structural properties is discussed. It is demonstrated that by adjusting the deposition conditions, the stress of the as-grown material can be varied from -145 to 60 MPa. Examples of poly SiGe micromachined devices, prepared at 650°C, are presented. It is shown that by using as-grown poly SiGe, it is possible to realize surface-micromachined suspended membranes having 0.6-μm-wide and 50-μm-long supports. The effect of the average stress and stress gradient on the mechanical stability of surface-micromachined structures is illustrated. Finally, the strain in poly SiGe is measured, and it is found to vary, according to the deposition conditions from -6.88×10^-4 to 3.6×10^-1 These values are compared to those measured for APCVD poly Si     

Experimental and thermodynamic study of tantalum-containing iron-based alloys reinforced by carbides: Part I — Case of (Fe,Cr)-based ferritic steels

Experiments and thermodynamic calculations were performed on three iron-based alloys containing 30 wt% of chromium and 3 to 6 wt% of tantalum. Solidus temperatures, natures, and surface fractions of all phases present after an exposure for 50 h at 1000, 1100, and 1200  ^°C, were determined for each alloy. These results were compared to values calculated using Thermo-Calc. Two alloys display solidus temperatures above 1400  ^°C, while all the liquidus temperatures are higher than 1500  ^°C. Tantalum carbides are present with high fractions, compared to similar Co-based and Ni-based alloys. Their observation and quantification using electron microscopy micrographs and image analysis may lead one to overestimate the surface fractions of TaC. Calculations of carbide fractions from the chemical composition of the matrix is to be preferred. A precipitation of coarse chromium carbides may occur for 1100 and 1200  ^°C.     

Influence of ambient temperature on OLED lifetime and uniformity based on modified equivalent lifetime detection

The ambient temperature can affect the OLED heat dissipation and aggravate the luminance degradation. Based on temperature‐related equivalent lifetime detection, a luminance compensation algorithm without internal or external sensing circuits is proposed and the influence of ambient temperature on lifetime and display uniformity is studied. First, the parameters of luminance degradation curves at any ambient temperature are calculated according to the relationship between accelerate degradation factor n and ambient temperature T, which is determined by the measured luminance degradation curves at ambient temperature 25°C, 45°C, and 80°C. Second, luminance compensation is carried out by increasing drive current according to the estimated luminance degradation influenced by temperature. Furthermore, compensation iterations m, compensation goal value L_goal, and compensation origin value L_origin are optimized to obtain a better lifetime extension at different ambient temperature. The simulated and experimental results indicate that the lifetime extensions considering the influence of ambient temperature at 0°C, 25°C, 45°C, 60°C, and 80°C are 29.7%, 28.1%, 18.7%, 18.9%, and 11.6%. Meanwhile, after displaying an image of the International Electrotechnical Commission (IEC) 62087 for 90 hours, the luminance uniformity of OLED increase to 96.0%, 94.0%, 97.2%, 97.2%, and 98.6%, which is a significant improvement compared with it of regardless the influence of the ambient temperature.     

High temperature stability of electrically conductive Pt–Rh/ZrO2 and Pt–Rh/HfO2 nanocomposite thin film electrodes

Nanocomposite films made up of either Pt–Rh/ZrO₂ or Pt–Rh/HfO₂ materials were co-deposited using multiple e-beam evaporation sources onto langasite (La₃Ga₅SiO₁₄) substrates, both as blanket films and as patterned interdigital transducer electrodes for surface acoustic wave sensor devices. The films and devices were tested after different thermal treatments in a tube furnace up to 1,200 °C. X-ray diffraction and electron microscopy results indicate that Pt–Rh/HfO₂ films are stabilized by the formation of monoclinic HfO₂ precipitates after high temperature exposure, which act as pinning sites to retard grain growth and prevent agglomeration of the conductive cubic Pt–Rh phase. The Pt–Rh/ZrO₂ films were found to be slightly less stable, and contain both tetragonal and monoclinic ZrO₂ precipitates that also helps prevent Pt–Rh agglomeration. Film conductivities were measured versus temperature for Pt–Rh/HfO₂ films on a variety of substrates, and it was concluded that La and/or Ga diffusion from the langasite substrate into the nanocomposite films is detrimental to film stability. An Al₂O₃ diffusion barrier grown on langasite using atomic layer deposition was found to be more effective than a SiAlON barrier layer in minimizing interdiffusion between the nanocomposite film and the langasite crystal at temperatures above 1,000 °C.     

A Sensing Device Using Liquid Crystal in a Micropillar Array Supporting Structure

We present the design of a micropillar array that leads to the formation of stable and uniform liquid crystal (LC) thin films for sensing applications. Photolithography and electroplating methods were employed to fabricate the micropillar array. By using this microfabricated structure, thin films of LC (5CB: 4'-pentyl-4-cyanobiphenyl) were formed and stabilized against gravitational forces and mechanical shock. The geometric profile of the supported LC thin film was simulated by using finite element methods. Orientational ordering transitions of nematic LCs in the supported thin films were used to detect liquid- and vapor-phase analytes via changes in the intensity of light transmitted through the LCs. The LC thin films supported by these microfabricated structures were tested and found to respond to dimethyl methylphosphonate gas.     

PECVD-SiOxNy films for large area self-sustained grids applications

In this work we study the structural properties and mechanical stress of silicon oxynitride (SiO_xN_y) films obtained by plasma enhanced chemical vapor deposition (PECVD) technique at low temperatures (320 °C) and report the feasibility of using this material for the fabrication of large area self-sustained grids. The films were obtained at different deposition conditions, varying the gas flow ratio between the precursor gases (N₂O and SiH₄) and maintaining all the other deposition parameters constant. The films were characterized by ellipsometry, by Fourier transform infrared (FT-IR) spectroscopy and by optically levered laser technique to measure the total mechanical stress. The results demonstrate that for appropriated deposition conditions, it is possible to obtain SiO_xN_y with very low mechanical stress, a necessary condition for the fabrication of mechanically stable thick films (up to 10 μm). Since this material (SiO_xN_y) is very resistant to KOH wet chemical etching it can be utilized to fabricate, by silicon substrate bulk micromachining, very large self-sustained grids and membranes, with areas up to 1 cm² and with thickness in the 2–6 μm range. These results allied with the compatibility of the PECVD SiO_xN_y films deposition with the standard silicon based microelectronic processing technology makes this material promising for micro electro mechanical system (MEMS) fabrication.     

Low temperature deposited titanium boride thin films and their application to surface engineering of microscale mold inserts

Titanium boride thin films were deposited at low temperatures by balanced magnetron sputtering and inductively coupled plasma (ICP) assisted balanced magnetron sputtering. The chemical composition, surface morphology, structure, and mechanical properties of titanium boride thin films were characterized by X-ray photoelectron spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy, and instrumented nanoindentation. As compared to titanium boride films deposited by balanced magnetron sputtering, the increase in plasma density surrounding the substrate surface during film growth afforded by the ICP assist causes significant film densification and mechanical property improvement. The morphology of titanium boride thin films deposited onto microscale non-flat Ta substrates and their effectiveness as barrier coatings for microscale compression molding of Al was characterized by focused ion beam sectioning and SEM. The present results show the potential of low-temperature deposited, conformal, titanium boride thin films for engineering surfaces of microscale mold inserts for microscale pattern replication in reactive metals by compression molding.     

基于湿热试验的光伏组件功率衰减与使用寿命研究

光伏组件功率衰减与使用寿命对于光伏电厂安全、经济运行具有重要意义。针对光伏组件功率衰减和使用寿命问题,在分析加速湿热条件下光伏组件归一化功率倒S形衰减规律基础上,提出以指数时间尺度变换函数对光伏组件非线性归一化功率进行变换,并运用Gamma过程对加速湿热条件下光伏组件归一化功率衰减数据进行建模,进而根据光伏组件使用寿命定义估计光伏组件使用寿命。通过加速湿热试验下光伏组件实测使用寿命与估计的使用寿命,验证了所提方法的正确性与合理性。方法表明,在50℃、45%相对湿度条件下光伏组件平均寿命近似为20~25年。与此同时,还对现有的加速退化试验进行了分析改进,探讨了运用步降加速退化试验代替传统的恒定应力加速退化试验的可能性。     

Thermal isolation of high-temperature superconducting thin filmsusing silicon wafer bonding and micromachining

Using a new micromachining technology, thermally isolated thin films of high-temperature superconductor have been microfabricated. The intended application for these structures is in infrared bolometers. A silicon wafer bonding process produces a low thermal mass island of single-crystal silicon on a silicon nitride membrane which provides thermal isolation. The silicon can act as a seed for the epitaxial growth of YBa₂Cu₃O₇ on a yttria-stabilized zirconia buffer layer. This paper describes the overall concept of the thermally isolated device, and demonstrates that the micromachined structure can be fabricated with high-quality superconducting films     

Elimination of post-release adhesion in microstructures usingconformal fluorocarbon coatings

The adhesion of polysilicon microstructures to their substrates is eliminated using a relatively conformal hydrophobic fluorocarbon (FC) coating grown in a field-free zone of a plasma reactor. Experiments show that the FC film deposition on top of the microstructure and on the underside was approximately 2:1. The FC coating is able to cover the entire underside of a 200×200 μm² plate, with a 20% deposition nonuniformity. The coating exhibits a contact angle of 110° and is able to prevent adhesion of cantilever beams and doubly supported beams to their substrates even after direct immersion in DI water. The durability of the coating was tested using an accelerated aging method, predicting a lifetime of greater than ten years at 150°C. Periodic wear tests indicate that the coating remains hydrophobic even after 10⁷ contact cycles     

Modelling and experimental validation of thin-film effects in thermopile-based microscale calorimeters

Calorimeters can be miniaturized to the point where they can be integrated into platforms such as micro-total analysis systems (μTAS) or lab-on-chip. Models of microscale calorimeters currently fail to account for variations of material properties known to be present in thin films. This study attempts to address this deficiency. Resistivity and absolute Seebeck coefficient of gold and nickel thin films were found to vary linearly with the inverse of film thickness in the submicron range. Thin-film thermopiles composed of gold and nickel were fabricated and their resistance and sensitivity were measured. Our results show that thin-film effects can introduce a 15% decrease in sensitivity (temperature-to-voltage conversion ratio) and a 30% decrease in resolution (smallest resolvable temperature difference). Introducing material properties variation with film thickness into models of thermopile performance resulted in improved estimates. Modelling results suggest that grain boundary scattering is a strong contributor to the observed film-thickness-related change of resistivity and Seebeck coefficient. These observations have implications for improving the design and fabrication of thermopile-based, and other microfabricated, microscale calorimeters.