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Manufacturable plastic microfluidic valves using thermal actuation


Karthik Pitchaimani,a Brian C. Sapp,b Adam Winter,b Austin Gispanski,a Toshikazu Nishida*b and Z. Hugh
Fan*ac
Received 18th May 2009, Accepted 24th July 2009
First published as an Advance Article on the web 7th August 2009
Published on 07 August 2009. Downloaded by Michigan Technological University on 24/10/2014 19:28:32.

DOI: 10.1039/b909742b

A low-cost, manufacturable, thermally actuated, plastic microfluidic valve has been developed. The
valve contains an encapsulated, temperature-sensitive fluid, which expands, deflecting a thin
elastomeric film into a fluidic channel to control fluid flow. The power input for thermal expansion
of each microfluidic valve can be controlled using a printed circuit board (PCB)-based controller, which
is suitable for mass production and large-scale integration. A plastic microfluidic device with such
valves was fabricated using compression molding and thermal lamination. The operation of the valves
was investigated by measuring a change in the microchannels ionic conduction current mediated
by the resistance variation corresponding to the deflection of the microvalve. Valve closing was also
confirmed by the disappearance of fluorescence when a fluorescent solution was displaced in the valve
region. Valve operation was characterized for heater power ranging from 36 mW to 80 mW. When
the valve was actuating, the local channel temperature was 10 to 19  C above the ambient temperature
depending on the heater power used. Repetitive valve operations (up to 50 times) have been
demonstrated with a flow resulting from a hydrostatic head. Valve operation was tested for a flow rate
of 0.334.7 mL/min.

Introduction developing microvalves utilizing materials more suitable for lab-


on-a-chip devices, including glass, poly(dimethylsiloxane)
Microfluidic devices have shown steady improvement since the (PDMS), and plastics. These microvalves were actuated using
pioneering papers were published almost two decades ago.1,2 either passive or active actuation mechanisms, including electric,
Their progress to-date has been summarized in recent reviews,3,4 magnetic, piezoelectric, pneumatic, thermal, and phase change.7
exemplified by developments made towards microfluidic large- For example, Beebe and co-workers developed pH-responsive
scale integration.5,6 An integrated microfluidic system often hydrogel valves for self-regulation of micro-flows8,9 while several
requires several fundamental components, including valves, research groups exploited the phase change property of paraffin
pumps, and mixers. The portability and manufacturability of at a higher temperature to obstruct fluid flow in micro-
these components has proven to be one of the hindrances in channels.1012 Bau et al. adopted a valve based on freezing and
realizing the potential of microfluidics.7 To address this chal- melting of a water slug to achieve flow control13 while Backhouse
lenge, we report on advances in the development of one and co-workers electrically controlled the phase change of
component, a self-contained microvalve. polyethylene glycol to achieve the integration of polymerase
Microvalves are one of the critical building blocks required to chain reactions and capillary electrophoresis.14
complete a successful microfluidic system. They carry out PDMS-based elastic membrane valves have been popular in
a variety of functions including containing fluids, regulating the last few years. Quakes research group reported the concept
flows, and isolating one region from another in a microfluidic in 2000,15 followed by several studies using thousands of inte-
system. As reviewed by Oh and Ahn,7 most of the earlier grated microvalves for high-throughput applications.1620 Quake
microvalves were fabricated in siliconthe default material for valves consist of three layers of PDMS. Pneumatic channels in
conventional micro-electro-mechanical systems (MEMS). These one layer are used to control the fluid channels in another layer
micro-machined microvalves were primarily used in silicon- through the elastic property of the middle layer PDMS. Quake
based MEMS devices. With explosive growth in the field of valves have been adopted by a number of researchers; some
microfluidics over the last decade, efforts have been made in modifications have also been reported.2128 However, these valves
have disadvantages as pointed out by Whitesides and coworkers:
a
Interdisciplinary Microsystems Group, Department of Mechanical and the bulky external accessories for pneumatic actuations make the
Aerospace Engineering, University of Florida, Gainesville, Florida, equipment cumbersome to users and not portable.21 In such
32611-6250, USA. E-mail: hfan@ufl.edu; nishida@ufl.edu; Fax: +352-
392-7303 systems, the microfluidic device is significantly dwarfed by the
b
Interdisciplinary Microsystems Group, Department of Electrical and off-chip controllers for the on-chip valves. As a result, there is
Computer Engineering, University of Florida, Gainesville, Florida, 32611- a need for microvalves with a self-contained actuation mecha-
6130, USA nism that can be controlled in a hybrid packaging platform
c
Department of Biomedical Engineering, University of Florida, Gainesville,
Florida, 32611-6131, USA
similar to the mother board in computers. Grover et al. also
Electronic supplementary information (ESI) available: Supplementary discussed another drawback of Quake valves:27 PDMS-based
Fig. S1. See DOI: 10.1039/b909742b valves are difficult to manufacture in industrial settings. In

3082 | Lab Chip, 2009, 9, 30823087 This journal is The Royal Society of Chemistry 2009
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addition, PDMS is incompatible with many reagents.29 This photolithography and wet chemical etching. By electroplating on
work intends to address both disadvantages by reporting on the the glass substrate, a nickel alloy mold was generated and then
design, fabrication, and characterization of microvalves actuated employed to produce plastic parts from COC resins (Zeonor
by a temperature-sensitive liquid heated with microfabricated 1020R) using a Carver hydraulic press (Wabash, IN). A CNC
thermal resistors. The resistors are addressed and individually milling machine was employed to trim the plastic parts into 1  3
powered by a printed circuit board (PCB) based controller, in. substrates and drill 2 mm-diameter wells at the channel ends.
a packaging technique currently used in the semiconductor and All channels in the microfluidic device were 110 mm wide and
Published on 07 August 2009. Downloaded by Michigan Technological University on 24/10/2014 19:28:32.

computer industry. A cyclic olefin copolymer (COC) was used 45 mm deep. After cleaning, the channel layer was ready for the
for fabricating the microfluidic devices and microvalves for its subsequent lamination step.
compatibility with chemical and biological applications. COC We used pressure sensitive adhesive tape 9019 (3M, Minne-
has been exploited by several research groups3034 for micro- apolis, MN) as the elastomeric film. According to the manufac-
fluidic studies and is commonly used in industry for turer, the tape is comprised of 13 mm-thick polyethylene
manufacturing compact discs and plastic lenses. terephthalate (PET) film coated with adhesive on both sides. The
The principle of the microvalve in this work is illustrated in tensile modulus of PET is (46)  105 psi.35 To laminate PET
Fig. 1. When heat is supplied to a temperature-sensitive fluid, with the channel layer, the liner from one side of the PET film
volumetric expansion of the fluid deflects an elastomeric film into was first removed. The film was laminated in a way to ensure firm
a microchannel. As a result, the channel is blocked and the valve contact with the channel layer. The two layer assembly was then
is closed. Heat input to the temperature-sensitive fluid is supplied left overnight to reach full bond strength.
through micro-fabricated heaters. The power supply to these The valve layer was made from 250 mm-thick Zeonor 1020R
heaters can be controlled using a PCB based controller. PCB- film from PLITEK (Des Plaines, IN). The film was cut into a size
controlled valve actuation will enable large scale integration of of 1  3 inch and drilled with 2 mm diameter holes at locations
these valves for high throughput applications and is also suitable where valve actuation was desired. After cleaning, the valve-layer
for industrial mass production. was laminated with the other adhesive side of the PET film that
had been assembled with the channel layer. The center of the
Experimental cavity in the valve-layer was aligned with the microfluidic
channel in the device. The assembled device was then left in clean
Device design and fabrication air to increase the adhesive bond strength. The geometry of the
Fig. 1a shows the schematic of a device consisting of four layers. valve cavity was chosen based on the expansion calculation as
The top layer contains microfluidic channels (channel layer). discussed below; the relationship between the cavity size and the
The second layer is an elastomeric film (elastomer layer). The fluidic channel geometry is expected to be studied in the future.
third layer contains cavities where a temperature-sensitive fluid is The heater layer is a 250 mm-thick Zeonor 1020R film
encapsulated (valve layer). The bottom layer is a plastic thin patterned with micro-heaters. To create micro-heaters,
a 1000 A -thick Au film was deposited onto a cleaned plastic film
film with patterned heaters (heater layer).
The channel layer was fabricated using the molding procedure by sputtering. Serpentine Au resistors were then obtained by
described previously.34 Briefly, a photomask pattern was photolithographic patterning and etching. The cleaned heater
designed using AutoCAD and then reproduced in glass using layer was then bonded with the previously assembled channel
layer-elastomeric film-valve layer. Solvent bonding was used
with decalin, following the procedure reported previously.36 The
solvent was introduced to the bonding areas only using the
microstamping approach.37 The assembly was then heated at
60  C for 20 min to complete the solvent bonding.

Temperature-sensitive fluid
3M Fluorinert FC40 (boiling point: 155  C) was selected as the
temperature-sensitive fluid.38 The cavity in the valve layer was
filled after the 4-layer device was assembled. An access hole was
drilled in the open space between the microheater traces in the
heater layer after patterning the micro-heaters. The location of
the hole was marked in the Au resistor pattern when it was
Fig. 1 (a) Schematic of a normally-open microfluidic valve consisting of designed. Since the cavity was very small (0.79 mL), a vacuum
four layers. The top channel layer contains microfluidic channels. The filling method was developed as follows. The device was
second layer is an elastomeric film. The third layer is a valve layer that
immersed in a Fluorinert solution in a beaker while the filling
houses a temperature-sensitive fluid. The bottom heater layer contains
hole was about 12 mm below the liquid level. This beaker was
resistive micro-heaters patterned on a cover film. When power is supplied
to the micro-heaters, the temperature-sensitive fluid expands, deflecting then placed in a vacuum desiccator, which was pumped down to
the elastomeric film into the channel. (b) The valve is closed after the 20 in. Hg pressure. The air in the cavity was replaced with Flu-
heater is turned on. (c) Three-dimensional cartoon showing 4-layer valve orinert when the vacuum was slowly released. The cavity filled
structure (note that it is upside down for easy visualization). The drawing with Fluorinert was inspected under a microscope, followed by
is not to scale. sealing with a tiny drop of RBC2001 epoxy (Warwick, RI).

This journal is The Royal Society of Chemistry 2009 Lab Chip, 2009, 9, 30823087 | 3083
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Valve operation challenges. The first one is to bond four layers of plastics
together. Initially, an all COC device structure using multiple-
After completing the assembly of the four-layer microvalve, the
bonded layers of COC was investigated. It showed partial actu-
inlet of the microchannel was constructed using an Upchurch
ation owing to the very low flexibility of the 100 mm-thick COC
Nanoport (Oak Harbour, WA), which was used for connecting
membrane and consequently needed a high operation tempera-
the microchannel to a pump. The contact pads of the micro-
ture. Therefore, we replaced the 100 mm-thick COC membrane
heater were connected to a custom PCB controller or directly to
layer with a 13 mm-thick PET film as discussed in the experi-
a 5 V power supply (Agilent E3644A, Santa Clara, CA). A
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mental section. The maximum elongation for COC is 3% whereas


solution of sodium chloride or a fluorescent dye was driven into
it is 60165% for PET according to the manufacturers data-
the channel by either hydrostatic head or a syringe pump (UMP-
sheets. The mechanical flexibility and thin thickness enable PET
II, World Precision Instruments, Inc. Sarasota, FL).
to function as an elastomeric film according to our experimental
The valve operation temperature was monitored using
results. The PET film also has appropriate bonding characteris-
a temperature sensor (a 76 mm diameter type K thermocouple
tics with both the channel layer and the valve layer. Solvent
from Omega), which was placed under the heater layer of the
bonding was used for the heater layer since it involves no
device. Four layers of Kapton tape were used to cover the sensor
microfluidic channels; thus concerns about possible channel
to minimize heat loss. In one experiment, an additional 50 mm
distortion and contamination do not exist.
diameter thermocouple was placed inside the microfluidic
The second challenge is to fabricate a micro-heater with the
channel or the Fluorinert solution in the heater cavity to corre-
appropriate resistance. After evaluating carbon ink, chromium,
late temperatures in different regions of the device.
SiO2/Cr, gold and tungsten, gold was selected due to its good
We measured the electric ionic conduction current in the
adhesion and uniform deposition onto plastics. Gold was
microfluidic channel to characterize valve operation since the
deposited on a COC film using sputtering, followed by photo-
total electrical resistance is proportional to the valve cross
lithographic patterning. The average resistance of the fabricated
sectional area if the microvalve resistance dominates the total
micro-heater was 222 U  12 U (N 36). The value of resistance
resistance. The channel was filled with 1 M or 0.1 M NaCl
was designed such that sufficient power can be supplied to the
solution. A constant voltage (8 V) was supplied between two ends
micro-heater to achieve reliable valve actuation using a 5 V
of the microfluidic channel via two platinum electrodes inserted
power supply. Fig. 2a shows a device with micro-heaters. The
into the channel inlet and outlet. The resulting electric ionic
relative thickness of three layers to the microchannel in the
current was measured by recording the voltage drop across
channel layer is illustrated in Fig. 2b.
a 56 kU resistor that was placed in series with the microfluidic
The third challenge is to fill a temperature-sensitive fluid in
channel. Measurement of the electric current, as well as the
a 0.79 mL cavity. Vacuum was used to facilitate filling of the fluid
thermocouple voltage was automated using Labview and
into the cavity as discussed in the experimental section. Fig. 2c
a multifunctional DAQ card NI-PCI 6229 (National Instru-
shows a micrograph of the top view of the cavity filled with the
ments, Austin, TX) with a SCC68 68-pin connector block and
fluid. Vacuum-filling often leaves a tiny air bubble in the cavity as
SCC-TC thermocouple signal processing module. The data
shown in Fig. 2c; the average size of the air bubble is about 6% of
acquisition sampling rate was set at 10 Hz.
the cavity volume. Note that the presence of the air bubble will
Fluorescence measurement not interfere with imaging capabilities of the device since the area
of interest is outside the valves (e.g., channels) after valves are
In addition to the electrical resistance, an optical method was characterized and optimized.
employed to verify valve actuation by monitoring fluorescence in
the channel. For the fluorescence measurement, a thermally lami-
nated 4 mil (100 mm) thick Topas 8007 film (PLITEK, Des Plaines,
IN) was used as the elastomeric film in the microvalve device.
Rhodamine B (0.1 mM, 20 mM carbonate buffer) was used to
replace NaCl solution in the microfluidic channel. Fluorescence
measurement was carried out using an inverted microscope (IX51,
Olympus, America Inc., Melville, NY), as discussed previously.39
Fluorescent images were acquired by a scientific-grade CCD digital
camera (C4742-80-12AG Hamamatsu, Bridgewater, NJ). The
channel walls were pre-treated to reduce residual fluorescent dye
adhesion to walls and surfaces. The surface treatment was per-
formed as follows:40 channels were first rinsed with pure water, then Fig. 2 (a) Picture of a plastic microfluidic device containing microvalves.
filled with 2% hydroxyethyl cellulose, 1% bovine serum albumin, Channels were filled with blue dye, and the valve cavities for the
and 1 tris-HCl tricine buffer, followed by rinsing with pure water. temperature-sensitive liquid were filled with red dye for easy visualiza-
tion. The device was sealed with a cover film patterned with Au micro-
heaters. (b) Picture of the cross-section of a device, showing the four-layer
Results and discussion structure. Only a portion of the channel layer is in the picture due to the
Valve fabrication field of view. (c) Exploded view of a micro-heater consisting of Au
serpentine resistors and a cavity filled with a temperature-sensitive fluid.
To fabricate a valve in a microfluidic device such as the four-layer The diameter of the cavity is 2 mm. It also shows the relative location of
structure described in Fig. 1, we must address three critical the filling hole and a microfluidic channel.

3084 | Lab Chip, 2009, 9, 30823087 This journal is The Royal Society of Chemistry 2009
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Operation temperatures the device geometry and the fluid used in this work. The calcu-
lation was based on the volumetric coefficient of thermal
The microvalves operation temperature is critical to its thermal
expansion, a,
actuation. It must be considerably lower than the glass transition
temperature of the plastic materials used (e.g., 105  C for Zeonor DV
a
1020R). In addition, the temperature in the microchannel should V ,DT
be less than the maximum temperature allowed by the sample of where V is volume and T is temperature. Values used for calcu-
interest (e.g., some enzymes denature at a temperature in excess of 
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lation include 0.0012 cm3/cm3 C for a of fluorinert, 0.79 mL for


50  C41). At the same time, the temperature must be high enough the cavity volume (V), and 0.0082 mL for the channel volume in
to expand the thermal-sensitive fluid sufficiently to close the the valve region (DV). However, the experimental results in Fig. 3
valve. As a result, we measured temperatures at various locations indicate that the required minimum temperature change of the
of the device when varying electrical power was applied to the thermal-sensitive fluid in the cavity was 27  C. The difference
micro-heater. Fig. 3 shows the temperatures as a function of from the calculated value is attributed to the additional expan-
power supplied. The temperature in the microchannel was sion required to bend the PET film, compression of the tiny air
measured by placing a thermocouple (50 mm-diameter) inside the bubble in the cavity, conductive heat losses to the plastic material
channel very close to the edge of the temperature-sensitive fluid of the device, and convective heat loss to the ambient.
cavity. The temperature of the Fluorinert fluid in the cavity was
higher than that in the channel due to the direct contact of the Valve actuation
Fluorinert fluid with the heater. The PET film between the Flu-
orinert fluid and the channel functions as a thermal insulator, The microfluidic channel was filled with a conductive solution
resulting in a lower steady-state temperature in the channel. (NaCl). A hydrostatic head of 9.5 mm at the inlet resulted in
Radial heat conduction away from the circular device axis and a flow rate of 333 nL/min, calculated using the HagenPoiseuille
heat loss to the ambient also helped to lower the channel flow.42 Valve operation was confirmed by measuring the electric
temperature. Also indicated in Fig. 3 is the temperature of ionic conduction current through the microchannel containing
a sensor placed under the heater layer. The concurrent measure- a valve.24,43 The minima in the conduction current through the
ment of temperatures at different locations enabled the use of the channel associated with the closure of the microvalve correlated
more easily placed external heater temperature sensor through well with the temperature in the heater cavity which drives the
the rest of this work due to convenience and its non-interference thermal actuation. As the temperature increased and the PET
with the valve operation. Four layers of Kapton tape were used to film deflected into the channel, a reduction in the local cross-
cover the temperature sensor to minimize heat loss. The highest sectional area increased the channel electrical (and fluidic)
power in Fig. 3 was selected so that all temperatures were at least resistance and decreased the electric current to zero. Fig. 4a
20  C below the glass transition temperature of Zeonor 1020R shows the temporal variation of the electric ionic conduction
and the lowest power in Fig. 3 corresponded to the minimum current in the channel as well as the temporal profile of the micro-
power required to actuate the valve. The results indicate that the heater temperature. A power of 75 mW was used in this experi-
local channel temperature was 10 to 19  C above the ambient ment. The cyclic valve actuation in Fig. 4a demonstrated the
temperature when the valve was actuating. These temperatures repeatability of valve operation.
generally do not affect reagents in most applications. The actuation of the microvalve was also confirmed by
The minimum temperature change of the thermal fluid observance of a reduction in the fluorescence intensity when the
required to actuate the valve was calculated to be 8.7  C based on channel was filled with a fluorescent solution. Fig. 4b shows
the change in the fluorescence intensity during valve action. The
elastomeric film displaced the fluorescent dye in the valve region,
resulting in a noticeable reduction in the fluorescent intensity.
Actuation of the microvalve at a variety of flow rates (from
0.89 to 4.7 mL/min) was studied. Different flow rates were ach-
ieved by using a range of hydrostatic pressure heads at the inlet.
Their temporal profiles of the electric current through the
microchannel are shown in the ESI Fig. S1, along with their
temporal profiles of the micro-heater temperature when the valve
was actuating. The results showed that the valve was operational
when the flow rate was as high as 4.7 mL/min. No leakage was
observed since the electric current through the channel was
reduced to zero in each case.

Actuation time

Fig. 3 Temperatures monitored at three positions, in the microchannel, The valve actuation time was expected to be shortened when
in the cavity housing a temperature-sensitive fluid, and adjacent to the a higher heater power was used since the time to achieve the
heater, are shown as a function of the heater power supplied. The inset necessary temperature change and thermal expansion of the
shows the approximate locations of thermocouples relative to the FC40 would be shorter. As a result, we studied the valve actu-
microvalve. ation time as a function of the input heater power (Fig. 5). The

This journal is The Royal Society of Chemistry 2009 Lab Chip, 2009, 9, 30823087 | 3085
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Fig. 6 Picture of a printed circuit board used to control thermally


actuated microvalves in a plastic microfluidic device. The board was
designed to control 16 valves. Also illustrated are the power source
connections, an interface to a computer, and the testing setup with one
microvalve in a plastic device.

hour. The results in Fig. 5 also indicate that the valve can be
Fig. 4 (a) Temporal profiles of the electric ionic conduction current operated over a wide range of power inputs. The valve actuation
through the microchannel (the Y axis on the right) and of the micro- time ranged from 780 s when power > 50 mW was used.
heater temperature (the Y axis on the left) when the valve was actuating. The results in Fig. 5 were obtained when the NaCl solution was
Three cycles of valve open and close are shown to illustrate repeatability. supplied by a hydrostatic head at 9.5 mm (333 nL/min as dis-
(b) Visualization of microvalve actuation using fluorescence in the cussed above). We also studied the valve operation when the
microchannel valve region before and after valve actuation. The channel
microfluidic channel was connected with a syringe pump. At
was filled with a fluorescent dye, rhodamine B. Some fibers present near
a flow rate of 300 nL/min (or 1.2 mm/s flow velocity), we
channel walls were absorbed with the fluorescent dye, however, they were
irrelevant with the valve actuation.
observed a similar phenomenon with a heater power of 65 mW
and 81 mW.

valve actuation time was calculated from the time when the
Integration
heater power was switched on to the time when the electric ionic
channel current decreased to a value less than 0.1% of the orig- For system applications, controlled thermal actuation of an
inal value and held that value for more than 5 s. Note that all array of microvalves is expected to be controlled by a PCB
experiments were performed under the same conditions controller using a packaging technique currently employed in the
described in the Experimental section. Other variables such as semiconductor and computer industry. Using PCB control of
flexibility of the elastomeric film and the flow rate in the micro- electrical heater power applied to thermally actuated microvalves
channel could play a role in the valve actuation time. We will eliminate the requirement of bulky accessories for pneu-
observed a considerable reduction in the actuation time when the matically actuated microvalves. PCB technology will also enable
power was increased initially. However, beyond a power of the large-scale integration of microfluidic valves for high-
50 mW up to 80 mW, the decrease in actuation time was less throughput applications.
pronounced which may be due to increasing thermal losses. For To illustrate the potential of using a PCB to control the power
each heater power value, except at the lowest power setting which supply to micro-heaters, a PCB controller was designed and
was at the threshold of actuation and highly variable, 6 to 8 valve constructed as shown in Fig. 6. The PCB consists of components
tests were conducted to obtain the standard deviation, which is mounted on an electrically insulating board including a micro-
indicated by the error bars. For the lowest power input (36 mW), processor, latches, and connectors; this PCB has the ability to
of the three tests, only one showed complete actuation while the control 16 microvalves. The dc 5 V may be supplied by either
remaining two had partial valve action in the time allotted of one a power supply or a computer. The actual power supplied to the
heater of a microvalve is controlled by a computer through the
PCB and a programmed graphic user interface. When a PCB
with one microvalve in a device was connected; similar results to
Fig. 4 were observed, showing the feasibility of the proposed
system integration.

Conclusion
We designed and fabricated a thermally actuated microvalve in
a plastic microfluidic device. Four layers of plastic sheets/films
were assembled together using lamination and solvent bonding.
Fig. 5 Valve actuation time as a function of input heater power. The The valve was actuated by a temperature-sensitive fluid that was
error bars indicated the standard deviation of multiple tests. heated using a microfabricated resistor. A thin PET film used in

3086 | Lab Chip, 2009, 9, 30823087 This journal is The Royal Society of Chemistry 2009
View Article Online

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This work is supported in part by Defense Advanced Research 6554.
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