Effect of trimethylsilane flow rate on the growth of SiC thin-films for fiber-optic temperature sensors

We have investigated the effect of trimethylsilane ([(CH/sub 3/)/sub 3/SiH] or 3MS) flow rate on the growth of SiC thin-film on single-crystal sapphire substrate for fiber-optic temperature sensor. The SiC film thickness was in the range of 2-3 /spl mu/m. The variation of the 3MS flow rate affected the structural properties of the SiC films. This, in turn, changed the optical properties and temperature sensing performance of the sensors. Optical reflection from the SiC thin-film Fabry-Pe/spl acute/rot interferometers showed one-way phase shifts in resonant minima on all measured samples. Linear fits to the resonant minima (at 660 to 710 nm) versus temperature provide the corresponding thermal expansion coefficient, /spl kappa//sub /spl phi//, of 1.7-1.9/spl times/10/sup -5///spl deg/C. With the optimized 3MS flow rate, the SiC temperature sensor exhibits a temperature accuracy of /spl plusmn/2.8/spl deg/C from 22 to 540/spl deg/C. The short-term SiC sensor stability at 532/spl deg/C for two weeks shows a very small standard deviation of 0.97/spl deg/C.     

Continuous flow polymerase chain reaction using a hybrid PMMA-PC microchip with improved heat tolerance

Recently, polymeric materials have been explored as more versatile alternatives for the fabrication of polymerase chain reaction (PCR) microchips. Poly(methyl methacrylate) (PMMA) is a popular substrate material due to its high mechanical stability, good chemical properties and most importantly, its suitability for cheap and simple CO₂ laser ablation. However, it has a low glass transition temperature (T_g) of 105 °C, which is just above the denaturation temperature for PCR, thus the bond integrity is compromised. Polycarbonate (PC) is preferred as a substrate for PCR microchip as it has a higher T_g of 150 °C; but since its thermal properties are not suitable for CO₂ laser light, the more expensive excimer laser has to be employed. Here we report a novel hybrid PMMA-PC microchip by bonding a PC cover plate with a PMMA substrate containing microchannel which is fabricated by CO₂ laser ablation. This hybrid microchip has improved heat tolerance, such that the bonding integrity is sustained at the denaturation temperature. DNA amplification is found to be more efficiently performed in a PMMA-PC microchip than in a PMMA-PMMA microchip.     

Liquid velocity distribution in slug flow in a microchannel

The liquid velocity distributions in two-phase slug flows in a nearly rectangular microchannel etched on a microfluidic chip were investigated using a three-dimensional tracking method for submicron fluorescent particles seeded in the working liquid (water). The Taylor bubbles generated from dissolved air in the water through heating the micro-fluidic chip to 35–55°C had low velocities, so they had the very small Capillary and Reynolds numbers. The change in the Taylor bubble shape with the flow conditions such as the bubble velocity and temperature was negligible in the present study. The shapes of the fully developed Taylor bubbles were determined by analyzing the interference fringes in in-line holographic images of the microchannel section containing the bubble to estimate the bubble cross-sectional area. The three-dimensional liquid velocity distribution for the two-phase slug flow was obtained using a least-squares fit of the measured tracer particle velocities to an analytic velocity distribution for Poiseuille flow in a rectangular channel to determine the mean liquid velocity and the liquid flow rate in the slug. The liquid velocity was normalized using the measured instantaneous bubble velocity to remove the influence of the slug and the bubble velocity fluctuations on the liquid velocity distribution. The results show that the mean liquid velocity through the microchannel corners is 2.3 times the bubble velocity, which is in agreement with previous observations of the maximum liquid velocity in the corners of 3.5–3.8 times the bubble velocity.     

High-performance temperature-programmed microfabricated gas chromatography columns

This paper reports the first development of high-performance, silicon-glass micro-gas chromatography (/spl mu/GC) columns having integrated heaters and temperature sensors for temperature programming, and integrated pressure sensors for flow control. These 3-m long, 150-/spl mu/m wide and 250-/spl mu/m deep columns, integrated on a 3.3 cm square die, were fabricated using a silicon-on-glass dissolved wafer process. Demonstrating the contributions to heat dissipation from conduction, convection, and radiation with and without packaging, it is shown that using a 7.5-mm high atmospheric pressure package reduces power consumption to about 650 mW at 100/spl deg/C, while vacuum packaging reduces the steady-state power requirements to less than 100 mW. Under vacuum conditions, 600 mW is needed for a temperature-programming rate of 40/spl deg/C/min. The 2300 ppm//spl deg/C TCR of the temperature sensors and the 50 fF/kPa sensitivity of the pressure sensors satisfy the requirements needed to achieve reproducible separations in a /spl mu/GC system. Using these columns, highly resolved 20-component separations were obtained with analysis times that are a factor of two faster than isothermal responses.     

Microheated substrates for patterning cells and controlling development

Here, we seek to control cellular development by devising a means through which cells can be subjected to a microheated environment in standard culture conditions. Numerous techniques have been devised for controlling cellular function and development via manipulation of surface environmental cues at the micro- and nanoscale. It is well understood that temperature plays a significant role in the rate of cellular activities, migratory behavior (thermotaxis), and in some cases, protein expression. Yet, the effects and possible utilization of micrometer-scale temperature fields in cell cultures have not been explored. Toward this end, two types of thermally isolated microheated substrates were designed and fabricated, one with standard backside etching beneath a dielectric film and another with a combination of surface and bulk micromachining and backside etching. The substrates were characterized with infrared microscopy, finite element modeling, scanning electron microscopy, stylus profilometry, and electrothermal calibrations. Neuron culture studies were conducted on these substrates to 1) examine the feasibility of using a microheated environment to achieve patterned cell growth and 2) selectively accelerate neural development on regions less than 100 /spl mu/m wide. Results show that attached neurons, grown on microheated regions set at 37/spl deg/C, extended processes substantially faster than those incubated at 25/spl deg/C on the same substrate. Further, unattached neurons were positioned precisely along the length of the heater filament (operating at 45/spl deg/C) using free convection currents. These preliminary findings indicate that microheated substrates may be used to direct cellular development spatially in a practical manner.     

Microfluidic patterning of nanoparticle monolayers

A microfluidic technique was developed to pattern nanoparticle monolayer controllably in a tentative polydimethylsiloxane (PDMS) microchannel. It was found that nanoparticle monolayer could be achieved in a two-step fluidic process: nanoparticle sedimentation and DI water rinsing. When nanoparticle suspension flows through a tentative PDMS microchannel, the particles will settle down due to the gravity effect and the Brownian motion and be captured onto the amino-functionalized substrate via electrostatic attraction. Aggregation on the substrate followed by a necessary DI water rinsing transforms hill-like nanoparticle aggregates into monolayer. Removing the tentative PDMS microchannel, pattern of nanoparticle monolayer following the channel shape was obtained. Experimental results indicated that the final monolayered nanoparticle coverage decreases when the flowing velocity in the sedimentation and/or the rinsing steps increases. Based on the continuity essence of fluid flow, different flowing velocities could be realized in one microchannel by varying the channel size. Therefore, monolayer patterns with controllable coverage could be achieved by carefully designing the microchannel width. The present approach is believed to be a promising nanoparticle monolayer patterning technique.     

A mold and transfer technique for lead-free fluxless soldering and application to MEMS packaging

This paper demonstrates a technique to premold and transfer lead-free solder balls for microelectrocmechanical systems (MEMS)/electronics packaging applications. A reusable bulk micromachined silicon wafer is used to mold a solder paste and remove excess flux prior to transfer to a host wafer that may contain released MEMS. This technique has been used to fabricate low temperature thin film MEMS vacuum packages. Long term (>5 months) reliability of these packages at room temperature and pressure is demonstrated through integrated Pirani gauges. These packages have survived over 600 hours in an autoclave (130/spl deg/C, 85% RH, 2 atm) and more than 1300 temperature cycles (55/spl deg/C to 125/spl deg/C).     

A low-temperature thin-film electroplated metal vacuum package

This paper presents a packaging technology that employs an electroplated nickel film to vacuum seal a MEMS structure at the wafer level. The package is fabricated in a low-temperature (<250/spl deg/C) 3-mask process by electroplating a 40-/spl mu/m-thick nickel film over an 8-/spl mu/m sacrificial photoresist that is removed prior to package sealing. A large fluidic access port enables an 800/spl times/800 /spl mu/m package to be released in less than three hours. MEMS device release is performed after the formation of the first level package. The maximum fabrication temperature of 250/spl deg/C represents the lowest temperature ever reported for thin film packages (previous low /spl sim/400/spl deg/C). Implementation of electrical feedthroughs in this process requires no planarization. Several mechanisms, based upon localized melting and Pb/Sn solder bumping, for sealing low fluidic resistance feedthroughs have been investigated. This package has been fabricated with an integrated Pirani gauge to further characterize the different sealing technologies. These gauges have been used to establish the hermeticity of the different sealing technologies and have measured a sealing pressure of /spl sim/1.5 torr. Short-term (/spl sim/several weeks) reliability data is also presented.     

Spatially resolved temperature measurement in microchannels

Non-intrusive local temperature measurement in convective microchannel flows using infrared (IR) thermography is presented. This technique can be used to determine local temperatures of the visualized channel wall or liquid temperature near this wall in IR-transparent heat sinks. The technique is demonstrated on water flow through a silicon (Si) microchannel. A high value of a combined liquid emissivity and substrate overall transmittance coupled with a low uncertainty in estimating this factor is important for quantitative temperature measurement using IR thermography. The test section design, and experimental and data analysis procedures that provide increased sensitivity of the detected intensity to the desired temperature are discussed. Experiments are performed on a 13-mm long, 50 μm wide by 135 μm deep Si microchannel at a constant heat input to the heat sink surface for flow rates between 0.6 and 1.2 g min⁻¹. Uncertainty in fluid temperature varies from a minimum of 0.60°C for a Reynolds number (Re) of 297 to a maximum of 1.33°C for a Re of 251.     

An electrostatic, on/off microvalve designed for gas fuel delivery for the MIT microengine

The MIT micro-gas turbine engine requires an integrated fuel-metering device in order to implement on-board engine control. Graded fuel control can be achieved with an array of on/off valves. Each valve in the array must withstand an annealing temperature of 1100/spl deg/C during fabrication and open against 1 MPa of supply pressure at 400/spl deg/C operating temperature. This paper presents the design, fabrication and testing of an electrostatic, on/off silicon prototype valve. Tested with nitrogen at room temperature, the valve opened against a differential pressure of 0.9 MPa with 136 V and delivered a mass flow rate of 45 sccm (3.38 g/h). At 0.1y MPa upstream pressure, the helium leak-rate was measured to be 6/spl times/10/sup -3/ sccm. The valve showed no sign of failure after being continuously actuated for more than 10/sup 5/ cycles. The prototype valve will serve as the base-line design for the engine fuel valve array.     

Electrokinetically driven flow control using bare electrodes

This paper presents a novel technique for manipulating fluid flows within microchannels using bare electrodes. The electrodes, with a width of 100 μm, are fabricated using conventional photolithography techniques by etching the bulk flow channel into a glass substrate and then depositing Pt/Cr thin films within this channel. The application of an external voltage to these electrodes produces localized variations in the electrical potential distribution, which in turn induce changes in the velocity and direction of the flow within the microchannel. The effectiveness of the proposed control technique is investigated numerically using computational fluid dynamics simulations and experimentally using a fabricated microchip containing multiple bare electrode-pairs. The results demonstrate that the application of appropriate driving voltages to the bare electrode-pairs enables the microdevice to function as a nozzle, a diffuser, a mixer or a valveless valve.     

New low-stress PECVD poly-SiGe Layers for MEMS

Thick poly-SiGe layers, deposited by plasma-enhanced chemical vapor deposition (PECVD), are very promising structural layers for use in microaccelerometers, microgyroscopes or for thin-film encapsulation, especially for applications where the thermal budget is limited. In this work it is shown for the first time that these layers are an attractive alternative to low-pressure CVD (LPCVD) poly-Si or poly-SiGe because of their high growth rate (100-200 nm/min) and low deposition temperature (520/spl deg/C-590/spl deg/C). The combination of both of these features is impossible to achieve with either LPCVD SiGe (2-30 nm/min growth rate) or LPCVD poly-Si (annealing temperature higher than 900/spl deg/C to achieve structural layer having low tensile stress). Additional advantages are that no nucleation layer is needed (deposition directly on SiO/sub 2/ is possible) and that the as-deposited layers are polycrystalline. No stress or dopant activation anneal of the structural layer is needed since in situ phosphorus doping gives an as-deposited tensile stress down to 20 MPa, and a resistivity of 10 m/spl Omega/-cm to 30 m/spl Omega/-cm. With in situ boron doping, resistivities down to 0.6 m/spl Omega/-cm are possible. The use of these films as an encapsulation layer above an accelerometer is shown.     

Flow control in microdevices using thermally responsive triblock copolymers

Active and passive microflow control has been demonstrated using gel formation by dilute aqueous solutions of triblock copolymers at elevated temperatures. Solutions of a poly(ethylene oxide)/sub 106/-poly(propylene oxide)/sub 70/-poly(ethylene oxide)/sub 106/ polymer, which has the trade name Pluronic/spl reg/ F127, have been used as a sample system. Flow in a microchannel has been stopped in less than 33 ms by introducing heat with an integrated electric heater. Viscous heating under high shear rates also induces gel formation, which has been used for passive automated flow control in a microchannel.     

Inner surface modification of poly(dimethylsiloxane) microchannel with chitin for electrophoretic analysis of proteins

Microchip electrophoresis in a poly(dimethylsiloxane) microfluidic device is one of the versatile separation techniques in a micro total analysis system, while an unstable electroosmotic flow depending on an inner surface of a microchannel and a nonspecific adsorption of biogenic compounds onto the inner surface are often problematic in microchip electrophoresis. To overcome these drawbacks, a chitin-coated poly(dimethylsiloxane) microchannel was newly developed by a relatively simple experimental procedure based on vacuum drying. The obtained chitin-coating showed high durability during 10-times experiments with a stable electroosmotic flow. It was also confirmed that the chitin-coated poly(dimethylsiloxane) microchannel provided the pH-dependent electroosmotic flow related to the dissociations of amino and silanol groups of chitin and poly(dimethylsiloxane), respectively. The nonspecific adsorption of fluorescently labeled proteins onto the inner surface of the channel was well suppressed by the coating, resulting in the sharp and symmetric peak without tailing in the microchip electrophoretic analysis of proteins. The separation of the proteins was also demonstrated in the chitin-coated microchannel, so that the resolution and reproducibility of the migration time were improved as compared to those in the untreated microchannel.     

Fabrication and measured performance of a first-generation microthermoelectric cooler

The measured performance of a column-type microthermoelectric cooler, fabricated using vapor-deposited thermoelectric films and patterned using photolithography processes, is reported. The columns, made of p-type Sb/sub 2/Te/sub 3/ and n-type Bi/sub 2/Te/sub 3/ with an average thickness of 4.5 /spl mu/m, are connected using Cr/Au/Ti/Pt layers at the hot junctions, and Cr/Au layers at the cold junctions. The measured Seebeck coefficient and electrical resistivity of the thermoelectric films, which were deposited with a substrate temperature of 130/spl deg/C, are -74 /spl mu/V/K and 3.6/spl times/10/sup -5/ /spl Omega/-m (n-type, power factor of 0.15 mW/K/sup 2/-m), and 97 /spl mu/V/K and 3.1/spl times/10/sup -5/ /spl Omega/-m (p-type, power factor of 0.30 mW/K/sup 2/-m). The cooling performance of devices with 60 thermoelectric pairs and a column width of 40 /spl mu/m is evaluated under a minimal cooling load (thermobuoyant surface convection and surface radiation). The average cooling achieved is about 1 K. Fabrication challenges include the reduction of the column width, implementation of higher substrate temperatures for optimum thermoelectric properties, and improvements of the top connector patterning and deposition.     

Characterization of low-temperature wafer bonding using thin-film parylene

This paper presents detailed experimental data on wafer bonding using a thin Parylene layer, and reports results on: 1) bond strength and its dependence on bonding temperature, bonding force, ambient pressure (vacuum), and time, 2) bond strength variation and stability up to two years post bond, and 3) bond strength variation after exposure to process chemicals. Wafer bonding using thin (<381 nm) Parylene intermediate layers on each wafer in a standard commercial bonder and aligner has been successfully developed. The Parylene bond strength is optimized at 230/spl deg/C, although Parylene bonding is possible at as low as 130/spl deg/C. The optimized bonding conditions are a low-temperature of /spl sim/230/spl deg/C, a vacuum of /spl sim/ 0.153 mbar, and 800 N force on a 100 mm wafer. The resultant Parylene bond strength is 3.60 MPa, and the strength for wafers bonded at or above 210/spl deg/C is maintained within 93% of its original value after two years. The bond strength is also measured after exposure to several process chemicals. The bond strength was reduced most in undiluted AZ400K (base) by 69% after one week, then in BHF (acid), MF319 (base), Acetone (solvent), and IPA (solvent) by 56%, 33%, 20%, and 8%, respectively, although less than one hour exposure to these chemicals did not cause a significant bond strength change (less than 11%). [1487].     

VHF single crystal silicon capacitive elliptic bulk-mode disk resonators-part II: implementation and characterization

This work, the second of two parts, reports on the implementation and characterization of high-quality factor (Q) side-supported single crystal silicon (SCS) disk resonators. The resonators are fabricated on SOI substrates using a HARPSS-based fabrication process and are 3 to 18 /spl mu/m thick. They consist of a single crystal silicon resonant disk structure and trench-refilled polysilicon drive and sense electrodes. The fabricated resonators have self-aligned, ultra-narrow capacitive gaps in the order of 100 nm. Quality factors of up to 46 000 in 100 mTorr vacuum and 26000 at atmospheric pressure are exhibited by 18 /spl mu/m thick SCS disk resonators of 30 /spl mu/m in diameter, operating in their elliptical bulk-mode at /spl sim/150 MHz. Motional resistance as low as 43.3 k/spl Omega/ was measured for an 18-/spl mu/m-thick resonator with 160 nm capacitive gaps at 149.3 MHz. The measured electrostatic frequency tuning of a 3-/spl mu/m-thick device with 120 nm capacitive gaps shows a tuning slope of -2.6 ppm/V. The temperature coefficient of frequency for this resonator is also measured to be -26 ppm//spl deg/C in the temperature range from 20 to 150/spl deg/C. The measurement results coincide with the electromechanical modeling presented in Part I.     

Evaluation of elastic properties and temperature effects in Si thin films using an electrostatic microresonator

Laterally driven microresonators were used to estimate the temperature-dependent elastic modulus of single-crystalline Si for microelectromechanical systems (MEMS). The resonators were fabricated through surface micromachining from silicon-on-glass wafers. They were moved laterally by alternating electrostatic force at a series of frequencies, and then a resonance frequency was determined, under temperature cycling in the range of 25/spl deg/C to 600/spl deg/C, by detecting the maximum displacement. The elastic modulus was obtained in the temperature range by Rayleigh's energy method from the detected resonance frequency. At this time, the temperature dependency of elastic modulus was affected by surface oxidation as well as its intrinsic variation: a temperature cycle permanently reduces the resonance frequency. The effect of Si oxidation was analyzed for thermal cycling by applying a simple composite model to the measured frequency data; here the oxide thickness was estimated from the difference in the resonance frequency before and after the temperature cycle, and was confirmed by field-emission scanning electron microscopy. Finally, the temperature coefficient of the elastic modulus of Si in the <110> direction was determined as -64/spl times/10/sup -6/[/spl deg/C/sup -1/]. This value was quite comparable to those reported in previous literatures, and much more so if the specimen temperature is calibrated more exactly.     

Design and characterization of an electrothermally driven monolithic long-stretch microdrive in compact arrangement

An electrothermally driven long stretch microdrive (LSMD) is presented for planar rectilinear motions in hundreds of micrometers. Design concept is based on connecting several actuation units in series to form a cascaded structure to accumulate relative displacement of each unit, and two cascaded structures are further arranged in parallel by a connection bar to double output force. The proposed area-saving design features monolithic compliant structure in compact arrangement to achieve long stroke. In experiments, the maximum reversible operating voltage is 3 V. In addition, the voltage-displacement relation shows good linearity within /spl plusmn/5% in 0.5-3.0 V. Fabricated nickel LSMD can generate displacement up to 215 /spl mu/m (W=8 /spl mu/m, /spl theta/=0.2/spl deg/, D=34 /spl mu/m) at 3 dc volts (669 mW). The maximum operation temperatures of tested LSMDs at 3 V are below 300 /spl deg/C. Output forces up to 495 /spl mu/N are measured by in situ passive micromechanical test beams. The LSMD can be operated at 100 Hz without degradation on displacement. Two geometrical design parameters, bent angle and constraint bar width, are also investigated analytically and experimentally.     

Evaluation of plasma deposited silicon nitride thin films for microsystems technology

Plasma deposited silicon nitride thin films were deposited at temperatures between 150/spl deg/C and 300/spl deg/C. Diagnostic microstructures were fabricated from the thin films using bulk micromachining, and the strain was calculated from optical measurement of postbuckling deflection. The results indicate that the residual strain of the thin films is dominated by film-substrate thermal mismatch, with the coefficient of thermal expansion monotonically increasing with decreasing deposition temperature. Metal-insulator-metal devices of variable area were also fabricated to measure the dielectric constant, which was shown to be independent of deposition temperature. The importance of these results to microsystems technology (MST) was briefly discussed.