Using silicon microfabrication technology, microchemical devices have been constructed for the purpose of conducting heterogeneously catalyzed multiphase reactions. The motivation behind the design, the fabrication approach, and the experimental characterization are presented for two classes of devices. The first design involves multiple parallel channels with integrated filter structures to incorporate standard catalytic materials. These catalysts are in the form of finely divided porous particles in a packed-bed arrangement. The second device involves the incorporation of porous silicon as a catalyst support, in the form of a thin layer covering microstructured channels. These microstructured channels simulate the structure of a packed bed and enhance mass transfer relative to an open channel. The ability to incorporate features at the tens-of-microns scale can reduce the mass-transfer limitations by promoting mixing and dispersion for the multiple phases. Directly integrating the catalyst support structures into the channels of the microreactor allows the precise definition of the bed properties, including the support's size, shape and arrangement, and the void fraction. Such a design would find broad applicability in enhancing the transport and active surface area for sensing, chemical, and biochemical conversion devices. Reaction rates for the gas-liquid-solid hydrogenation of cyclohexene using the integrated catalyst with porous silicon as a support compare favorably to those rates obtained with the packed-bed approach. In both cases, the mass transfer coefficient is at least 100 times better than conventional laboratory reactors.

Design and fabrication of microfluidic devices for multiphase mixing and reaction

In this paper, anodic bonding between silicon wafer and glass wafer (Pyrex 7740) has been achieved at low temperature. The bond strength is measured using a tensile testing machine. The interfaces are examined and analyzed by scanning acoustic microscopy (SAM), scanning electron microscopy (SEM) and secondary ion mass spectrometry (SIMS). The effects of the bonding parameters on bond quality are investigated using the Taguchi method. The bonding temperature used ranges from 200 °C to 300 °C. Almost bubble-free interfaces have been obtained. The bonded area increases with increasing bonding temperature. The unbonded area is less than 1.5% within the whole wafer for bonding temperature between 200 °C and 300 °C. The bond strength is higher than 10 MPa and increases with the bonding temperature. Fracture mainly occurs inside the glass wafer other than in the interface when the bonding temperature is higher than 225 °C. Higher bonding temperature results in more oxygen migration to the interface and more Si–O bonds. The bonding mechanisms consist of hydrogen bonding and Si–O chemical reaction.

https://iopscience.iop.org/article/10.1088/0960-1317/13/2/308/pdf

Low temperature wafer anodic bonding

Microfabrication of analytical devices is currently of growing interest and many microfabricated instruments have also entered the field of mass spectrometry (MS). Various (atmospheric pressure) ion sources as well as mass analyzers have been developed exploiting microfabrication techniques. The most common approach thus far has been the miniaturization of the electrospray ion source and its integration with various separation and sampling units. Other ionization techniques, mainly atmospheric pressure chemical ionization and photoionization, have also been subject to miniaturization, though they have not attracted as much attention. Likewise, all common types of mass analyzers have been realized by microfabrication and, in most cases, successfully applied to MS analysis in conjunction with on-chip ionization. This review summarizes the latest achievements in the field of microfabricated ion sources and mass analyzers. Representative applications are reviewed focusing on the development of fully microfabricated systems where ion sources or analyzers are integrated with microfluidic separation devices or microfabricated pums and detectors, respectively. Also the main microfabrication methods, with their possibilities and constraints, are briefly discussed together with the most commonly used materials.

Microchip technology in mass spectrometry.

When a femtosecond laser pulse is focused at the interface of two transparent substrates, localised melting and quenching of the two substrates occur around the focal volume, bridging them due to nonlinear absorption. The substrates can then be joined by resolidification of the materials. We investigate the optimum irradiation conditions needed to join borosilicate glass substrates and fused silica substrates using a 1 kHz 800 nm Ti:sapphire amplifier. We characterised the joint strength and the transmittance through joint volumes as a function of laser energy and translation velocity. We found that a joining strength as large as 14.9 MPa could be obtained in both fused silica and borosilicate glass. Annealing the joint samples led to an increase in the joint strength.

Direct joining of glass substrates by 1 kHz femtosecond laser pulses

This paper introduces a simplified fabrication method for vacuum-sealed capacitive micromachined ultrasonic transducer (CMUT) arrays using anodic bonding. Anodic bonding provides the established advantages of wafer-bondingbased CMUT fabrication processes, including process simplicity, control over plate thickness and properties, high fill factor, and ability to implement large vibrating cells. In addition to these, compared with fusion bonding, anodic bonding can be performed at lower processing temperatures, i.e., 350°C as opposed to 1100°C; surface roughness requirement for anodic bonding is more than 10 times more relaxed, i.e., 5-nm rootmean- square (RMS) roughness as opposed to 0.5 nm for fusion bonding; anodic bonding can be performed on smaller contact area and hence improves the fill factor for CMUTs. Although anodic bonding has been previously used for CMUT fabrication, a CMUT with a vacuum cavity could not have been achieved, mainly because gas is trapped inside the cavities during anodic bonding. In the approach we present in this paper, the vacuum cavity is achieved by opening a channel in the plate structure to evacuate the trapped gas and subsequently sealing this channel by conformal silicon nitride deposition in the vacuum environment. The plate structure of the fabricated CMUT consists of the single-crystal silicon device layer of a silicon-on-insulator wafer and a thin silicon nitride insulation layer. The presented fabrication approach employs only three photolithographic steps and combines the advantages of anodic bonding with the advantages of a patterned metal bottom electrode on an insulating substrate, specifically low parasitic series resistance and low parasitic shunt capacitance. In this paper, the developed fabrication scheme is described in detail, including process recipes. The fabricated transducers are characterized using electrical input impedance measurements in air and hydrophone measurements in immersion. A representative design is used to demonstrate immersion operation in conventional, collapse-snapback, and collapse modes. In collapsemode operation, an output pressure of 1.67 MPa pp is shown at 7 MHz on the surface of the transducer for 60-Vpp, 3-cycle sinusoidal excitation at 30-V dc bias.

A three-mask process for fabricating vacuum-sealed capacitive micromachined ultrasonic transducers using anodic bonding

Anodic bonding between Si-based and glass substrates has been characterized in detail. The effects of magnitude of the applied voltage, surface properties (coating of Si substrate), and surface cleanliness (pre-bonding cleaning procedure) on the time required for complete bonding were thoroughly studied. First, the generic bonding time versus applied voltage plot was found to be concave in shape (viewed from the origin). For bonding between p-type Si substrate and Corning 7740 glass pre-cleaned with acetone, the time required was cut down from 38 to 4 min if the applied voltage was increased from 200 to 500 V. Second, the bonding time required for five Si-based substrates in ascending order was determined to be Si (p-type), polysilicon, silicon nitride, silicon oxide and then Si (n-type). Third, the bonding between p-type Si substrate, pre-cleaned with H2SO4–H2O2 and HF, and Corning 7740 glass was completed within 1 min, which was much faster than that pre-cleaned with acetone (4 min). Finally, from bonding point of view, Corning 7740 glass was superior to Corning 7059 glass and Fisher slide due to its thermal coefficient of expansion matching with the underlying Si substrate and the presence of significant amount of sodium ions in the glass.

Connie Y.N. Liaw

Papers

Detailed characterization of anodic bonding process between glass and thin-film coated silicon substrates