A micromachining process is described for fabricating a mass spectrometry electrospray source on a silicon chip. The process utilizes polymer (parylene) layers to form a system of chambers, filters, channels, and hollow needle structures (electrospray emitters) that extend more than a millimeter beyond the edge of the silicon substrate. The use of photoresist as the sacrificial layer facilitates the creation of long channels. Access to the channel structures on the chip is through a port etched through the silicon substrate that also serves as a sample reservoir. A reusable chip holder consisting of two plastic plates and an elastomer gasket provides the means to mount the chip in front of the mass spectrometer inlet and make electrical and gas connections. The electrospray emitters have tapered tips with 5 microns x 10 microns rectangular openings. The shape of the tip can be varied depending on the shape of the mask used to protect the parylene structures during the final plasma etch. The parylene emitters are physically robust and require only a high electric field to achieve stable electrospray operation over a period of a few hours. Direct comparisons with conventional glass or fused silica emitters indicated very similar performance with respect to signal strength and stability, spectral quality, and endurance. The automated MS/MS analysis of a mixture of tryptic peptides was no more difficult and yielded nearly identical results as the analysis of the same sample using a conventional nanospray device. This work demonstrates that an efficient electrospray interface to mass spectrometry can be integrated with other on-chip structures and mass-produced using a batch process.
Two generations of check-valved silicone rubber diaphragm pumps are presented. Significant improvements have been made from pump to pump including the design and fabrication of a double-sided check valve, a bossed silicone membrane, and silicone gaskets. Water flow rates of up to 13 ml/min and a maximum back pressure of 5.9 kPa were achieved through pneumatic operation with an external compressed air source. Using a custom designed solenoid actuator, flow rates of up to 4.5 ml/min and a maximum back pressure of 2.1 kPa have been demonstrated.
We present here the first surface-micromachined, normally closed, in-channel, Parylene check valve (Fig. 1). This device is fabricated monolithically on a silicon substrate using a five-layer Parylene process. The operating structure of the check valve is a circular sealing plate on top of a ring-shaped valve seat. The sealing plate is center-anchored on top of a chamber diaphragm that is vacuum-collapsed to the bottom of the chamber in order to achieve a normally closed position. A thin gold layer on the roughened valve seat surface is used to reduce stiction between the sealing plate and the valve seat. We have achieved an in-channel check valve with a cracking (opening) pressure of 20-40 kPa under forward bias and no measurable leakage under reverse bias up to 270 kPa. Using this design, this valve performs well in two-phase microfluidic systems (i.e. microchannel flows containing gas, liquid, or gasfliquid mixture).
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