Stefan Schlautmann

Room-temperature intermediate layer bonding for microfluidic devices

In this work a novel room-temperature bonding technique based on chemically activated Fluorinated Ethylene Propylene (FEP) sheet as an intermediate between chemically activated substrates is presented. Surfaces of silicon and glass substrates are chemically modified with APTES bearing amine terminal groups, while FEP sheet surfaces are treated to form carboxyl groups and subsequently activated by means of EDC-NHS chemistry. The activation procedures of silicon, glass and FEP sheet are characterized by contact angle measurements and XPS. Robust bonds are created at room-temperature by simply pressing two amine-terminated substrates together with activated FEP sheet in between. Average tensile strengths of 5.9 MPa and 5.2 MPa are achieved for silicon-silicon and glass-glass bonds, respectively, and the average fluidic pressure that can be operated is 10.2 bar. Moreover, it is demonstrated that FEP-bonded microfluidic chips can handle mild organic solvents at elevated pressures without leakage problems. This versatile room-temperature intermediate layer bonding technique has a high potential for bonding, packaging, and assembly of various (bio-) chemical microfluidic systems and MEMS devices.

One-step sculpting of silicon microstructures from pilars to needles for water and oil repelling surfaces

Surfaces that repel both water and oil effectively (contact angles > 150°) are rare. Here we detail the microfabrication method of silicon surfaces with such properties. The method is based on careful tuning of the process conditions in a reactive etching protocol. We investigate the influence of SF6, O2 and CHF3 gases during the etching process using the same pitch of a photolithographic mask. Varying the loading conditions during etching, we optimized the conditions to fabricate homogeneous pedestal-like structures. The roughness of the microstructures could also effectively be controlled by tuning the dry plasma etching conditions. The wetting behavior of the resulting microstructures was evaluated in terms of the water and oil contact angles. Excitingly, the surfaces can be engineered from superhydrophobic to omniphobic by variation of the aforementioned predefined parameters

Disposable Attenuated Total Reflection-Infrared Crystals from Silicon Wafer: A Versatile Approach to Surface Infrared Spectroscopy

Attenuated total reflection-infrared (ATR-IR) spectroscopy is increasingly used to characterize solids and liquids as well as (catalytic) chemical conversion. Here we demonstrate that a piece of silicon wafer cut by a dicing machine or cleaved manually can be used as disposable internal reflection element (IRE) without the need for polishing and laborious edge preparation. Technical aspects, fundamental differences, and pros and cons of these novel disposable IREs and commercial IREs are discussed. The use of a crystal (the Si wafer) in a disposable manner enables simultaneous preparation and analysis of substrates and application of ATR spectroscopy in high temperature processes that may lead to irreversible interaction between the crystal and the substrate. As representative application examples, the disposable IREs were used to study high temperature thermal decomposition and chemical changes of polyvinyl alcohol (PVA) in a titania (TiO(2)) matrix and assemblies of 65-450 nm thick polystyrene (PS) films.

Glucose level determination with a multi-enzymatic cascade reaction in a functionalized glass chip

In this work we show the functionalization of the interior of microfluidic glass chips with poly(2-hydroxyethyl methacrylate) polymer brushes as anchors for co-immobilization of the enzymes glucose-oxidase and horseradish peroxidase. The formation of the brush layer and subsequent immobilization of these enzymes have been characterized on flat surfaces by atomic force microscopy and Fourier transform infrared spectroscopy, and studied inside glass chips by field emission scanning microscopy. Enzyme-functionalized glass chips have been applied for performing a multi-enzymatic cascade reaction for the fast (20 s) determination of glucose in human blood samples and the result is in excellent agreement with values obtained from the conventional hospital laboratory. The limit of detection of this bi-enzymatic method is 60 μM. With the advantages of high selectivity and reproducibility, this functionalization method can be used for improving the efficiency of glucose sensors.

A Supramolecular Sensing Platform for Phosphate Anions and an Anthrax Biomarker in a Microfluidic Device

A supramolecular platform based on self-assembled monolayers (SAMs) has been implemented in a microfluidic device. The system has been applied for the sensing of two different analyte types: biologically relevant phosphate anions and aromatic carboxylic acids, which are important for anthrax detection. A Eu(III)-EDTA complex was bound to β-cyclodextrin monolayers via orthogonal supramolecular host-guest interactions. The self-assembly of the Eu(III)-EDTA conjugate and naphthalene β-diketone as an antenna resulted in the formation of a highly luminescent lanthanide complex on the microchannel surface. Detection of different phosphate anions and aromatic carboxylic acids was demonstrated by monitoring the decrease in red emission following displacement of the antenna by the analyte. Among these analytes, adenosine triphosphate (ATP) and pyrophosphate, as well as dipicolinic acid (DPA) which is a biomarker for anthrax, showed a strong response. Parallel fabrication of five sensing SAMs in a single multichannel chip was performed, as a first demonstration of phosphate and carboxylic acid screening in a multiplexed format that allows a general detection platform for both analyte systems in a single test run with μM and nM detection sensitivity for ATP and DPA, respectively.

Electrokinetic sorting and collection of fractions for preparative capillary electrophoresis on a chip

A microfabricated device capable of selecting and collecting multiple components from a mixture separated by capillary electrophoresis (CE) is described. This collection is automated and can be easily controlled by a set of rules defined by an operator, enabling fast and consistent operation. The device consists of an electrokinetically steered fluidic network that can be divided into three sections: a CE part, a fractions distribution region and a set of storage channels. Sample fractions leave the CE channel and are detected in the interfacial region by fluorescence intensity measurements. If an upcoming peak is detected, separation is withheld and the potentials are reconfigured to force the fraction into one of the collection channels, where they become available for further processing or analysis. The sequence of separation and collection is repeated until all the bands of interest are captured. A mixture of three fluorescent dyes (Rhodamine 6G, Rhodamine B and Fluorescein) was used to demonstrate the principle. The components were repeatedly separated by means of CE and pooled in their respective storage channels. In comparison to previous developments, the system presented in this paper offers automatic collection of all fractions in a single run. Furthermore, it is possible to run the system in a repetitive mode for accumulative pooling if more fractionated sample is required.

In-line sample concentration by evaporation through porous hollow fibers and micromachined membranes embedded in microfluidic devices

Two types of microfluidic systems, a porous hollow fiber and a thin supported membrane with an array of micromachined holes, are investigated for concentrating mass‐limited analyte samples. Water evaporation is driven by the partial pressure difference across the hydrophobic membrane, induced by dry sweeping gas on the permeate side. An analytical model permitting clarification of the contribution of design and process parameters on acquisition of concentrated solution and prediction of achievable concentration factors is presented. Concentrating an exemplary solution utilizing the two systems has been studied at different experimental conditions to validate the model. The results show that the hollow fiber gives controllable concentration factors of more than 10. For the micromachined membrane concentrator concentration factors of 6–8 were achieved, at much lower flow rates than predicted by the model. Because of the asymptotic dependence of concentration factor on flow rate, accurate control of the liquid feed is extremely critical in the flow rate range where high concentration factors are obtained, and the smallest variations in liquid flow rate may easily lead to supersaturation and deposition of solutes in the pores. This changes membrane porosity in an unpredictable way and limits the maximum attainable concentration factor.

Chip-Based Multicapillary Column with Maximal Interconnectivity to Combine Maximum Efficiency and Maximum Loadability

On the basis of our previous work on the design of pillar array columns for liquid chromatography, we report on a new pillar array design for high-efficiency, high volumetric loadability gas chromatography columns. The proposed pillar array configuration leads to a column design which can either be considered as a packed bed with perfectly ordered and uniform flow paths or as multicapillary columns (8 parallel tracks) with a maximal interconnectivity between the flow paths to avoid the so-called polydispersity effect (dispersion arising from the inevitable differences in migration velocity between parallel flow paths). Despite our relative inexperience with column coating, and most probably (not supported by data) suffering from the same problem of stationary phase pooling in the right-angled corners of the flow-through channels as other chip-based GC devices, the efficiencies obtained in a L = 70 cm long and 75 μm deep and 6.195 mm wide chip for, respectively, quasi-unretained and retained components (k = 7) went up to N = 60 000 and 12 500 under isothermal conditions using H2 as carrier gas and a downstream restriction. Under programmed temperature conditions (Ti = 80 °C, Tf = 175 °C at 30 °C/min, and a H2 flow of 0.4 mL/min), a peak capacity of 170 was obtained in 3.6 min. For retained compounds, the optimal flow rate is found to be on the order of 0.4 mL/min, achieved at an operating pressure of 2.3 bar. Intrinsically, the column combines the efficiency of a 75 μm capillary with the volumetric loadability of a 240 μm capillary.

Continuous-wave laser generated jets for needle free applications

We designed and built a microfluidic device for the generation of liquid jets produced by thermocavitation. A continuous wave (CW) laser was focused inside a micro-chamber filled with a light-absorbing solution to create a rapidly expanding vapor bubble. The chamber is connected to a micro-channel which focuses and ejects the liquid jet through the exit. The bubble growth and the jet velocity were measured as a function of the devices geometry (channel diameter D and chamber width A). The fastest jets were those for relatively large chamber size with respect to the channel diameter. Elongated and focused jets up to 29 m/s for a channel diameter of [Formula: see text] and chamber size of [Formula: see text] were obtained. The proposed CW laser-based device is potentially a compact option for a practical and commercially feasible needle-free injector.

Toward jet injection by continuous-wave laser cavitation

Abstract. This is a study motivated by the need to develop a needle-free device for eliminating major global healthcare problems caused by needles. The generation of liquid jets by means of a continuous-wave laser, focused into a light absorbing solution, was studied with the aim of developing a portable and affordable jet injector. We designed and fabricated glass microfluidic devices, which consist of a chamber where thermocavitation is created and a tapered channel. The growth of a vapor bubble displaces and expels the liquid through the channel as a fast traveling jet. Different parameters were varied with the purpose of increasing the jet velocity. The velocity increases with smaller channel diameters and taper ratios, whereas larger chambers significantly reduce the jet speed. It was found that the initial position of the liquid–air meniscus interface and its dynamics contribute to increased jet velocities. A maximum velocity of 94±3  m/s for a channel diameter of D=120  μm, taper ratio n=0.25, and chamber length E=200  μm was achieved. Finally, agarose gel-based skin phantoms were used to demonstrate the potential of our devices to penetrate the skin. The maximum penetration depth achieved was ∼1  mm, which is sufficient to penetrate the stratum corneum and for most medical applications. A meta-analysis shows that larger injection volumes will be required as a next step to medical relevance for laser-induced jet injection techniques in general.