• No results found

The microfluidics integration of gold-on-silicon nitride membranes was performed by mechanical engineering team as the project of Carlos Escobedo.

Fig. Cl shows the components of the microfluidic chip with integrated flow-through nanohole arrays. A 1.6 mm diameter hole was milled on a commercial glass slide. The gold-on-silicon nitride film was fixed to the holed glass slide using NOA

81 optical adhesive (Norland, Cranbury, NJ). A polydimethylsiloxane (PDMS) chip was fabricated using a replica molding technique reported elsewhere [141]. A master was fabricated by spin-coating SU-8 50 photoresist (MicroChem Corp., Newton, MA)

onto a clean 3 inch silicon wafer (Silicon Quest International Ine, Santa Clara, CA).

The mask used to create the microfluidic pattern, consisted of a 4 mm center reservoir and two 1.5 mm reservoirs for tubing access, all interconnected by a 200 µp? wide microchannel. The mask was placed over the coated wafer and exposed to UV light

¦/¦

Figure Cl: Schematic of the chip assembly showing the integration of nanohole arrays in gold-on-silicon nitride with microfluidics.

for 120 seconds and post-baked for 5 min. at 95 0C. The exposed wafer was devel-oped using SU-8 developer (MicroChem Corp., Newton, MA) and then hard baked at 65 0C for 1 minute and at 95 0C for 12 minutes. A degassed mixture of Sylgard 184 elastomer (Dow Corning, Midland, MI) and its curing agent at a 13:1 ratio was molded on the master. A separate PDMS layer was cast in a Petri dish with a clean silicon wafer to create a solid 1 mm thick PDMS spacer. After baking at 85 0C for 20 minutes, the replica and the spacer were removed from the molds. Two 1 mm holes for tubing connection and a centered 6 mm hole for fluid access were punched in the microfluidic replica and in the spacer, respectively. The replica and the spacer were exposed to oxygen plasma and irreversible bonded. The resulting assembly was irreversibly bonded to the holed glass slide with the fixed film.

Valve

Figure C. 2: Schematic of the experimental setup to facilitate flow-through nanohole

arrays.

Fig. C. 2 shows a schematic of the experimental setup for fluid delivery to and through the nanohole arrays. On one side, a syringe pump, a shut-off inlet valve and the PDMS chip were connected via 1/16 OD Fluorinated Ethylene Propylene tubing.

On the other side, a valve was connected to the chip outlet and the regulator of an Argon (Ar) tank. The syringe pump was used to fill the reservoir below the silicon nitride side of the nanohole arrays via the microfluidic chip. To drive fluid through the nanohole arrays at controlled pressure, the argon tank was used. While the gold-on-Si3N4 membranes proved very effective at supporting pressures required for flow-through operation, care was required to avoid damaging the membrane. Specifically, uncontrolled pressures generated by inserting or removing fluidic connections to an otherwise sealed chip could rupture the membrane.

For the fluorescein flow-through visualization tests, a chip assembly containing 15x15 µ??2 nanohole arrays with periodicities of 450 nm and hole diameters of 300 nm, 280 nm, 270 nm, 260 nm and 250 nm was used. The Au-coated side of the membrane

faced towards the 1Ox microscope objective. Fig. 5.9(b) shows a microscope image of six arrays of nanoholes, and a test pattern (TP) as lighter regions near the center of the image. The microfluidic circuit was opened by disconnecting the tubing at the barb connector and the chip was filled with filtered 1 mM fluorescein aqueous solution via the syringe pump. The syringe-side valve was then shut and the tubing reconnected at the barb connector with the outlet valve in off position. The nanohole arrays were then visualized using the epi-fluorescent microscope and CCD camera. To facilitate wetting, 3 µ\ of ethanol was in the hole in the glass slide of the chip assembly.

The Ar tank regulator was set to a pressure of 10 psi and the corresponding valve opened. Immediately after, images were acquired at a rate of 2 frames per second and exposure time of 343 ms. The images were 1324x1024 pixels and had an 8-bit dynamic range. The fluorescent solution streams observed exiting from the nanohole arrays end entered the ethanol environment, as shown in Fig. 5.9(c). The subsequent

movement of the streams was due to thermal and surface tension related currents in

the much larger ethanol environment. In an all microfluidic/nanofluidic environment these oscillations would not be present.

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