A microreactor for hydrogen production in micro fuel cell applications

A silicon-chip based microreactor has been successfully fabricated and tested for carrying out the reaction of methanol reforming for microscale hydrogen production. The developed microreactor in combination with a micro fuel cell is proposed as an alternative to conventional portable sources of electricity such as batteries due to its ability to provide an uninterrupted supply of electricity as long as a supply of methanol and water can be provided. The microreformer-fuel cell combination has the advantage of not requiring the tedious recharging cycles needed by conventional rechargeable lithium-ion batteries. It also offers significantly higher energy storage densities, which translates into less frequent "recharging" through the refilling of methanol fuel. The microreactor consists of a network of catalyst-packed parallel microchannels of depths ranging from 200 to 400 /spl mu/m with a catalyst particle filter near the outlet fabricated using photolithography and deep-reactive ion etching (DRIE) on a silicon substrate. Issues related to microchannel and filter capping, on-chip heating and temperature sensing, introduction and trapping of catalyst particles in the microchannels, flow distribution, microfluidic interfacing, and thermal insulation have been addressed. Experimental runs have demonstrated a methanol to hydrogen molar conversion of at least 85% to 90% at flow rates enough to supply hydrogen to an 8- to 10-W fuel cell.     

A magnetic bead-based DNA extraction and purification microfluidic device

This article introduces a novel magnetic bead-based DNA extraction and purification device using active magnetic mixing approach. Mixing and separation steps are performed using functionalised superparamagnetic beads suspended in cell lysis buffer in a circular chamber that is sandwiched between two external magnetic coils. Non-uniform nature of magnetic field causes temporal and spatial distribution of beads within the chamber. This process efficiently mixes the lysis buffer and whole blood in order to extract DNA from target cells. Functionalized surface of the magnetic beads then attract the exposed DNA molecules. Finally, DNA-attached magnetic beads are attracted to the bottom of the chamber by activating the bottom magnetic coil. DNA molecules are extracted from magnetic beads by washing and re-suspension processes. In this study, a circular PMMA microchamber, 25 μL in volume, 500 μm in depth and 8 mm in diameter was fabricated to purify DNA from spiked bacterial cell cultures into the whole blood sample using Promega Magazorb DNA extraction kit. The lysis efficiency was evaluated using a panel of Gram-positive (Bacillus subtilis) and Gram-negative (Escherichia coli) bacterial cells cultures into the blood sample to achieve approximately 100,000 copy levels inside the chip. Manufacturer’s standard extraction protocol was modified to a more simplified process suitable for chip-based extraction. The lysis step was performed using 5 min incubation at 56 °C followed by 5 min incubation at room temperature for binding process. Temperature rise was generated and maintained by the same external magnetic coils used for active mixing. The yield/purity and recovery levels of the extracted DNA were evaluated using quantitative UV spectrophotometer and real-time PCR assay, respectively. Real-time PCR results indicated efficient chip-based bacterial DNA extraction using modified extraction protocol comparable to the standard bench-top extraction process.     

基于纳米磁珠技术的新型微全分析DNA芯片的研究

在微全分析系统的研究中,样品提取及DNA分析技术是非常重要的一个环节.也是目前国内外研究的热点之一.文中介绍了一种新型的基于单芯片的样品制备和扩增方法.采用多层微加工技术制作SU-8模具,通过注模成型,制作出有立体微柱结构的PDMS(聚二甲基硅氧烷)芯片,在芯片微池内填充超顺磁性磁珠,利用固相提取(solid phase extraction,SPE)法,将细胞裂解、DNA提取、PCR反应等功能集成在一个PDMS芯片上.整个流程快速有效,操作简便且易于芯片系统集成,提取产物可以不必洗脱,直接作为下一步PCR反应的模板,在同一芯片上进行扩增反应,实现了样品预处理、DNA提取和PCR扩增的集成.     

Planar microreactor for biochemical application made from silicon and polymer films

Recently the progress of life science has been increasing rapidly, and the importance of the microfluidics for DNA analysis systems has been widely recognized, especially in medical fields. The polymerase chain reaction (PCR) is an essential technique for DNA assay of various diseases and it has been a strong requirement to shorten the total of PCR cycles more and more. We developed the microreactor with a single cell for PCR using fabrication technologies of MEMS. The reactor body and cover were sealed using high thickness PDMS prototyping film without using adhesive in order to achieve repeat grabbing motion for direct sample injection, resumption and cleansing the reaction cell. Good reproducibility of the heat cycling was obtained. The heating rate and cooling rate during PCR was 6.8 and 2.7°C, respectively, which well corresponds to the design parameters. The homogenous temperature distribution of variance less than 2.0°C was obtained. It is demonstrated that amplification of the DNA was successfully achieved by using the microreactor.     

Characterizations of VO2-based uncooled microbolometer linear array

Vanadium dioxide (VO₂) thin films are materials for uncooled microbolometer due to their high temperature coefficient of resistance (TCR) at room temperature. This paper describes the design and fabrication of eight-element uncooled microbolometer linear array using the films and micromachining technology. The characteristics of the array is investigated in the spectral region of 8–12 μm. The fabricated detectors exhibit responsivity of over 10 kV/W, detectivity of approximate 1.94×10⁸ cm Hz^1/2/W, and thermal time constant of 11 ms, at 300 K and at a frequency of 30 Hz. Furthermore, the uncorrected response uniformity of the linear array bolometers is less than 20%.     

Manufacture and characterization of sol–gel V1−x−yWxSiyO2 films for uncooled thermal detectors

V_1−x−yW_xSi_yO₂ films for uncooled thermal detectors were coated on sodium-free glass slides with sol–gel process, followed by the calcination under a reducing atmosphere (Ar/H₂ 5%). The V_1−x−yW_xSi_yO₂ films as prepared inherit various phase transition temperatures ranging from 20 to 70 °C depending on the dopant concentrations and the fabrication conditions. Compared to the hysteresis loop of plain VO₂ films, a rather steep loop was obtained with the addition of tungsten components, while a relaxed hysteresis loop with the tight bandwidth was contributed by Si dopants. Furthermore, the films with switching temperature close to room temperature were fabricated to one-element bolometers to characterize their figures of merit. Results showed that the V_0.905W_0.02Si_0.075O₂ film presented a satisfactory responsivity of 2600 V/W and detectivity of 9 × 10⁶ cm  Hz^1/2/W with chopper frequencies ranging from 30 to 60 Hz at room temperature. It was proposed that with appropriate amount of silicon and tungsten dopants mixed in the VO₂, the film would characterize both a relaxed hysteresis loop and a fair TCR value, which effectively reduced the magnitude of noise equivalent power without compromising its performance in detectivity and responsivity.     

A biocompatible Parylene thermal flow sensing array

A microelectromechanical systems (MEMS) thermal flow sensing array constructed of biocompatible materials has been designed, fabricated, and tested. In addition to the construction, the electronic biasing conditions were selected such that sensor operation was compatible with biological fluids. The device comprises several thin film platinum sensing elements sandwiched in a Parylene C membrane. The membrane is suspended over a bulk-micromachined silicon channel for improved thermal isolation. This sensing array layout permits, for the first time, operation in multiple flow sensing modes using a single device. Multi-mode testing was performed in hot-film, calorimetric, and time-of-flight modes at low overheat ratios. Furthermore, constant current (CC) and constant temperature (CT) biasing methods were explored in hot-film mode. The results of the various testing modes were compared and flow sensing down to 0.5 μL/min has been demonstrated.     

The assessment of heat radiation

Approximately 900 climatic chamber experiments were performed with 16 male subjects to study the thermal strain at climates including increased heat radiation. Based on the reactions of heart rate, rectal temperature and sweat rate, a heat stress index was developed for the assessment of climates with effective heat radiation intensities up to 1400 W m⁻². The index considers different combinations of dry air temperature (5–55°C), globe temperature (25–76°C), mean radiant temperature (25–160°C), air velocity (0.5–2.0 m s⁻¹), clothing, physical work load and directions of radiation and air flow.

The index integrates combinations of the variables producing the same degree of thermal strain into a single value. This value indicates the temperature of the physiologically equivalent climate in which air and radiant temperature are equal. It can be determined from a simple formula or from correspondent graphs.

In comparison, the international recommended heat stress indices are less capable to evaluate heat radiation correctly. The incorporation of the new partial index into the used indices may improve substantially their physiological validity in the assessment of climates with radiant heat stress.

Relevance to industry

The goal of this paper is to provide an improved assessment of thermal stress in working environments in which heat radiation is an important heat stress factor.     

Bead-based polymerase chain reaction on a microchip

We present a bead-based approach to microfluidic polymerase chain reaction (PCR), enabling fluorescent detection and sample conditioning in a single microchamber. Bead-based PCR, while not extensively investigated in microchip format, has been used in a variety of bioanalytical applications in recent years. We leverage the ability of bead-based PCR to accumulate fluorescent labels following DNA amplification to explore a novel DNA detection scheme on a microchip. The microchip uses an integrated microheater and temperature sensor for rapid control of thermal cycling temperatures, while the sample is held in a microchamber fabricated from (poly)dimethylsiloxane and coated with Parylene. The effects of key bead-based PCR parameters, including annealing temperature and concentration of microbeads in the reaction mixture, are studied to achieve optimized device sensitivity and detection time. The device is capable of detecting a synthetically prepared section of the Bordetella pertussis genome in as few as 10 temperature cycles with times as short as 15?min. We then demonstrate the use of the procedure in an integrated device; capturing, amplifying, detecting, and purifying template DNA in a single microfluidic chamber. These results show that this method is an effective method of DNA detection which is easily integrated in a microfluidic device to perform additional steps such as sample pre-conditioning.     

Self-assembly of three dimensional micro mechanisms using thermal shrinkage of polyimide

This paper describes three-dimensional microstructures fabricated using a simple self-assembly process involving the thermal shrinkage of polyimide. The proposed method enables hinged structures to be automatically rotated out of the wafer plane and to remain bent without the need to use any interlocking mechanisms. The hinged structures were fabricated using surface micromachining techniques involving heating in a furnace. An increase in the bending angle due to the shrinkage of polyimide was observed with increasing heating temperature, heating time, and length of the polyimide hinge. Of these three parameters, the heating time was found to be the most suitable for precise control of the bending angle. Furthermore, microcubes were fabricated by this method and the self-assembly process was successfully visualized using a CCD camera.     

Operator-based nonlinear temperature control experiment for microreactor group actuated by Peltier devices

In this paper, operator-based nonlinear water temperature control for a group of three connected microreactors actuated by Peltier devices is proposed. To control the water temperature of tube in the microreactor, the temperature change of aluminum effects is considered. Therefore, the temperature change of aluminum becomes the part of an input of the tube. First, nonlinear thermal models of aluminum plates and tubes that structure the microreactor are obtained. Then, an operator based nonlinear water temperature control system for the microreactor is designed. Finally, the effectiveness of the proposed models and methods is confirmed by simulation and experimental results.     

Fast transient temperature operating micromachined emitter for mid-infrared optical gas sensing systems: design, fabrication, characterization and optimization

A novel micromachined thermal emitter for fast transient temperature operation is presented. Compared to most commercial available thermal emitters, the one here presented is able to operate in a pulsed mode. This allows the use of lock-in techniques or pyrodetectors in the data acquisition without the use of an optical chopper for light modulation. Therefore, these types of thermal emitters are very important for small filter photometers. Several hot-plate suspension concepts were studied in order to find a design with excellent mechanical stability and high thermal decoupling. In contrary to the classical spider suspension design, a novel approach based on a non-axis-symmetric design is presented. The thermal emitters are fabricated using silicon on insulator technology and KOH-etching. The emitters are heated with Pt-meanders. For temperature determination an additional Pt-structure is deposited onto the hot-plates. The emitters are mounted in TO-5 housings using a ceramic adhesive and gold wire bonding. The used operation temperature is 750°C. In pulsed operation it’s important to have a large modulation depth in terms of thermal radiation intensity in the needed spectral range. The maximal reachable modulation depth ranges from ambient temperature to steady state temperature. A modulation frequency of 5 Hz still allows using nearly the maximum modulation depth. A parameterized finite element model was realized and adapted to the measured data. This was the basis for the numerical optimization procedure for a new improved design.     

Neisseria Meningitidis Detection Based on a Microcalorimetric Biosensor With a Split-Flow Microchannel

This paper proposes and demonstrates a novel microcalorimetric sensor for detecting Neisseria meningitidis. To eliminate additional heating structures and calibration steps, a split-flow microchannel is integrated into the microcalorimeter. The split-flow microchannel constantly maintains the output of the microcalorimeter near a zero level without the use of any heating elements when there is no biochemical reaction. With the use of the split-flow microchannel, an active heating element such as a heater is no longer required. In addition, to improve the sensitivity of the microcalorimeter, a thermal sensing component, which is a thermopile in this case, has been fabricated on a high thermal resistivity layer, which reduces the parasitic heat transfer to the silicon substrate and concentrates the released thermal energy to the thermopile. The characteristics of the proposed microcalorimeter were investigated by measuring the reaction heat of the biotin-streptavidin pairs. The sensitivity of the microcalorimeter was measured to be 0.21 V/cal. Then, a biological reaction between Neisseria meningitidis group B (NMGB) and its antibody was detected by using the proposed microcalorimeter. In order to verify the reliability of the measurement, exactly the same number of NMGB was reacted with its antibody and an optical density was measured by an enzyme-linked immunosorbent assay as a known reference.     

Potentiometric CO2 gas sensor with lithium phosphorous oxynitride electrolyte

Potentiometric cell, Au/LiCoO₂ 5 m/o Co₃O₄/Li_2.88PO_3.73N_0.14/Li₂CO₃/Au, has been fabricated and investigated for monitoring CO₂ gas. A LiCoO₂–Co₃O₄ mixture was used as the solid-state reference electrode instead of a reference gas. The idea is to keep the lithium activity constant on the reference side using thermodynamic equilibrium at a given temperature. The thermodynamic stability of the reference electrode was studied from the phase stability diagram of Li–Co–C–O system. The Gibb’s free energy of formation of LiCoO₂ was estimated at 500°C from the measured value of the cell emf. The sensors showed good reversibility and fast response toward changing CO₂ concentrations from 200 to 3000 ppm. The emf values were found to follow a logarithmic Nernstian behavior in the 400–500°C temperature range. CH₄ gas did not show any interference effect. Humidity and CO gas decreased the emf values of the sensor slightly. NO and NO₂ gases affect this sensor significantly at low temperatures. However, increased operating temperature seems to reduce the interference.     

Fabrication of ceramic microcomponents and microreactor for the steam reforming of ethanol

Ceramics have several advantages over other materials in MEMS, such as heat resistance, hardness, corrosion resistivity even in harsh environments, chemical inertness for biological applications and catalytic activity of surfaces and so on. For these advantages ceramic microstructures will be very potentially useful in microsystem, especially in microreactor. A novel method for the high aspect ratio micro ceramic structures fabrication based on deep X-ray lithography and lost-mold technique is developed. By using this method, ceramic microreactors have been successfully fabricated. The ceramic microreactor consists of 14 identical microchannels in parallel, each with typical dimensions of approximately 300 μm in width, 400 μm in height and 20 mm in length. The Ni film catalyst with thickness of 300 nm is uniformly coated through sputtering process. The steam reforming of Ethanol into hydrogen on the ceramics microreactor was studied at temperatures between 500 and 700°C. The microreactors have been characterized by studying of C₂H₆O conversion, H₂ selectivity, and product stream composition.     

Microstructure, electrical and ethanol-sensing properties of perovskite-type SmFe0.7Co0.3O3

Ultrafine SmFe_0.7Co_0.3O₃ powder, prepared by a sol–gel method, shows a single-phase orthogonal perovskite structure. The influence of annealing temperature upon its crystal cell volume, microstructure, electrical and ethanol-sensing properties was investigated in detail. When the annealing temperature increases from 600 to 950 °C, the unit cell volume of the SmFe_0.7Co_0.3O₃ sample reduces, and its average grain size increases. When the annealing temperature increases from 600 to 850 °C, the optimal working temperature and response to ethanol of the SmFe_0.7Co_0.3O₃ sensor increase, and the response–recovery time shortens. But when the annealing temperature further increases from 850 to 950 °C, there are decreases of the optimal working temperature and sensor response, and the response–recovery time is prolonged. The results indicate that, as for sensor response, its optimal annealing temperature is about 850 °C, and the sensor based on SmFe_0.7Co_0.3O₃ annealed at 850 °C shows the highest response S = 80.8 to 300 ppm ethanol gas, and it has the best response–recovery and selectivity characteristics. When the ethanol concentration is as low as 500 ppm, the curve of its optimal response versus concentration is nearly linear. Meanwhile, the influence mechanisms of annealing temperature upon the conductance, the optimal working temperature and sensor response for SmFe_0.7Co_0.3O₃ were studied.     

Microprobe array with electrical interconnection for thermalimaging and data storage

In this work, new novel methods for fabricating a thermal probe array with 32 × 32 probes on one chip are proposed. It consists of silicon micromachined probe, AlN actuator, pyramidal SiO₂ tip on which the nano-scale metal-metal junction is formed using a self-alignment technique. The nano-junction can be used as a thermocouple to measure a local temperature on a sample surface or as a nano-heater to make a local deformation on a media. Using the fabricated thermal probe, temperature distribution is measured on a prepared sample surface and the local heating capability of the thermal probe is confirmed. Preliminary experiments for data writing and reading are performed on a phase change medium     

Thermal measurement and analysis of micro hotplate array using thermography

A micro hotplate (MHP) array was made by incorporating several MHPs into a single chip as an integrated sensor array. The sensing film must operate at a specific high temperature condition (300–400 °C) with a low power consumption. In addition, each hotplate should be independent and all the hotplates should be uniform thermally. Therefore, the thermal characteristics of the individual hotplate must be measured. In this work, the temperature distribution in a 2×2 MHP array was measured using infrared thermography. The temperature distribution of the small area and other thermal characteristics were obtained, providing reliable experimental information for the design of the MHP array.     

Simulation and characterization of microreactors for aerosol generation

This paper shows the application of T-shaped micromixers for the generation of aerosols with nanoscale droplets by the mixing of a hot vapor–gas mixture with a cold gas. The fast mixing within a T-shaped micromixer leads to a high supersaturation of the vapor and therefore to an instantaneous, homogeneous nucleation and particle growth. Different mixer geometries, mixing ratios, and gas temperatures have been investigated by numerical simulation to yield optimum mixing results over a wide range of operational parameters. Optimized microreactor geometries were designed and fabricated in silicon with Pyrex glass lids. Special attention was paid to thermal insulation and particle deposition at the channel walls. This concerns not only the mixing chip, but also the design of the fluidic mount with only few bends and corners. Initial experimental results for particle deposition and aerosol generation are presented. High temporal temperature gradients up to 10⁶ K/s lead to a rapid condensation and forming of nanosized particles with a mean diameter of 20–50 nm and a narrow size distribution.