Download as pdf or txt
Download as pdf or txt
You are on page 1of 10

Electrowetting-based valve for the control of the capillary flow

Wataru Satoh, Hiroomi Yokomaku, Hiroki Hosono, Noriyuki Ohnishi, and Hiroaki Suzuki

Citation: Journal of Applied Physics 103, 034903 (2008); doi: 10.1063/1.2832629


View online: http://dx.doi.org/10.1063/1.2832629
View Table of Contents: http://scitation.aip.org/content/aip/journal/jap/103/3?ver=pdfcov
Published by the AIP Publishing

Articles you may be interested in


A pneumatic valve controlled microdevice for bioanalysis
Biomicrofluidics 7, 054116 (2013); 10.1063/1.4826158

Control of an electrowetting-based beam deflector


J. Appl. Phys. 107, 063101 (2010); 10.1063/1.3319649

Autonomous microfluidic transport using electrowetting-based valves and integrated cells


Appl. Phys. Lett. 95, 204105 (2009); 10.1063/1.3263956

Capillary filling in centrifugally actuated microfluidic devices with dynamically evolving contact line motion
J. Appl. Phys. 105, 084904 (2009); 10.1063/1.3110016

Capillary pinching in a pinched microchannel


Phys. Fluids 19, 033101 (2007); 10.1063/1.2709704

[This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP:
131.187.254.4 On: Sat, 22 Nov 2014 22:11:04
JOURNAL OF APPLIED PHYSICS 103, 034903 共2008兲

Electrowetting-based valve for the control of the capillary flow


Wataru Satoh, Hiroomi Yokomaku, Hiroki Hosono, Noriyuki Ohnishi, and Hiroaki Suzukia兲
Graduate School of Pure and Applied Sciences, University of Tsukuba, Tsukuba, Ibaraki 305-8573,
Japan
共Received 30 May 2007; accepted 18 November 2007; published online 6 February 2008兲
The behavior of a microfluidic device based on transport by capillary action and control by direct
electrowetting was examined by changing the device parameters. The device was constructed with
a polydimethylsiloxane 共PDMS兲 substrate with a flow channel and a glass substrate with electrodes
to control electrowetting. The microfluidic transport and valve action could be explained by
Washburn’s model, which suggests that the model can be used for designing such a device. The
device could be used for the timely delivery of a solution into many flow channels as well as for the
mixing of solutions. © 2008 American Institute of Physics. 关DOI: 10.1063/1.2832629兴

I. INTRODUCTION phenomenon alone, and a valve to control the movement of


the liquid column is necessary. However, the use of a valve
To construct highly sophisticated micro-total-analysis with a complicated structure nullifies the advantage resulting
systems or labs-on-a-chip, the integration of active microflu- from the spontaneous microfluidic transport and should lead
idic functions still remains a critical issue. In the current to malfunction by contamination.
trend, the volume of solutions handled in these devices is To take full advantage of the nature of the hydrophilic
steadily decreasing to the nanoliter or picoliter order. In the flow channel, electrowetting probably provides the most suit-
present microsystems, two representative methods mostly able principle of operation.3 Electrowetting is a phenomenon
used for microfluidic transport are electro-osmosis and pres- which features a change in the wettability of a metal surface
sure driving by external macroscopic pumps. However, these in response to a change in the applied potential. By combin-
methods have limitations. In electro-osmotic transport, a ing capillary action and electrowetting, efficient transport of
large power source is required to generate a high driving a solution and intentional control of the direction of flow are
voltage 共usually in the order of hundreds or thousands of realized. Although valves based on this principle have al-
volts兲. In addition, the transport of a solution in an empty ready been used and basic theoretical considerations target-
flow channel is impossible. With pressure driving, the trans- ing microfluidic applications have been reported,4–8 no sys-
port of a solution becomes difficult as the dimensions of the tematic directions for the design of the valves have been
flow channel decrease, particularly when hydrophobic parts provided. In this study, the movement of a liquid column in a
exist in the flow channel. Furthermore, the techniques for the microflow channel and a valve area was examined, and suit-
integration of pumps and valves have not yet been estab- able structures were considered on the basis of a theoretical
lished. So far, successful attempts have been observed in a analysis. Furthermore, the principle was also used for the
limited number of cases.1,2 delivery of a solution and the mixing of two solutions.
The ultimate microfluidic system will be one in which
solutions are efficiently transported in microflow channels II. EXPERIMENTAL
with minimum power consumption. This will become more
critical as the level of integration increases. From a practical A. Materials and reagents
point of view, the repetitive use of an analytical device for The materials used for fabrication and performance char-
real samples is often unrealistic because of the contamination acterization were obtained from the following commercial
of channel walls or other microfluidic components. There- sources: glass wafers 共No. 7740; 3 in. diameter, 500 ␮m
fore, the device structure and the principle of operation thickness兲, from Corning Japan 共Tokyo, Japan兲; a thick-film
should preferably be as simple as possible. To this end, the photoresist 共SU-8兲, from MicroChem 共Newton, MA兲, a pre-
use of capillary action is attractive. The capillary action fea- cursor solution of PDMS 共KE-1300T兲, from Shin-Etsu
tures spontaneous movement of a solution and does not re- Chemical 共Tokyo, Japan兲; and fluorescein and glycerol, from
quire any external power sources. Therefore, it is very attrac- Wako Pure Chemical Industries 共Osaka, Japan兲. Bovine se-
tive in systems of the microscopic scale, in which the rum albumin 共BSA兲 was obtained from the Sigma-Aldrich
influence of interfacial tension becomes more dominant. Re- Corporation 共Saint Louis, MO兲. Standard solutions were pre-
cent reports on this topic clearly point out the expectations pared with distilled-deionized water.
regarding the principle of operation. Needless to say, a con-
trollable microfluidic system cannot be constructed using this B. Movement of a liquid column in a flow channel

a兲 The movement of a solution in a capillary has been ex-


Author to whom correspondence should be addressed. Telephone: ⫹81-
298-53-5598. FAX: ⫹81-298-53-4490. Electronic mail: plained under different assumptions.9–12 Moreover, an accu-
hsuzuki@ims.tsukuba.ac.jp. rate solution for the Navier-Stokes equation for a rectangular

0021-8979/2008/103共3兲/034903/9/$23.00 103, 034903-1 © 2008 American Institute of Physics


[This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP:
131.187.254.4 On: Sat, 22 Nov 2014 22:11:04
034903-2 Satoh et al. J. Appl. Phys. 103, 034903 共2008兲

flow channel has been obtained.13 However, in designing a be replaced with 共2h + w兲␥LV cos ␪PDMS + w␥LV cos ␪glass for a
device, a simple formula is preferred if it does not cause flow channel surrounded by three walls of PDMS and one
serious errors. Our first objective was to test the applicability wall of glass. Consequently, an equation that corresponds to
of the Washburn equation9 Eq. 共1兲 is obtained,13,17,18

ẋ =
R
4␩x
␥LV cos ␪ . 共1兲 ẋ = 冉 冊冋
␥LV hw
8␩x h + w
2
2 cos ␪PDMS cos ␪PDMS + cos ␪glass
w
+
h
. 册
Here, ẋ is the flow velocity, R, the radius of a circular cap- 共8兲
illary, ␩, the viscosity of the solution, x, the distance from Here, ␪PDMS and ␪glass are the contact angles on PDMS and
the inlet of the capillary to the meniscus of the moving liquid glass. A similar equation is obtained from Eq. 共6兲 by using
column, ␥LV, the interfacial tension between the solution and ␪Au instead of ␪glass and by replacing only 2 cos ␪PDMS / w
the capillary wall, and ␪, the contact angle of the solution on with 2 cos ␪PDMS / w⬘. Here, w⬘ and ␪Au are the width of the
the walls. valve area and the contact angle on the gold electrode, re-
To lay the basis for later discussion, we begin with the spectively.
equation of motion from which the Washburn equation has Since the liquid column is moving, the contact angles
been derived10 used in the equations should be dynamic contact angles.16
d兵␳␲R2xẋ其 Even if dynamic contact angle should be taken into account,
= 2␲R␥LV cos ␪ − 8␲␩xẋ. 共2兲 we consider here only static contact angle which does not
dt
lead to significant errors 共see discussion below兲 and has the
Here, ␳ is the density of the solution. We solve Eq. 共2兲 under advantage to simplify discussions on design rules.
initial conditions of x = x0 and ẋ = 0 at t = 0. In the case treated
here, x0 is assumed to be very small but finite.14,15 By inte- C. Structure and fabrication of the test devices
grating the equation, we obtain

冉 冊
Test devices of three different structures were fabricated
R␥LV cos ␪
ẋ = 兵1 − exp共− t/␶兲其 for characterization. In the experiments to examine the
4␩ movement of a liquid column in a flow channel, the device

冋 冉
⫻ x 02 + 2
R␥LV cos ␪
4␩

兵t + ␶ exp共− t/␶兲 − ␶其 册 −1/2
.
shown in Fig. 1共a兲 was used. A straight rectangular flow
channel was formed with PDMS along with an injection port
and an air vent. The flow channel was formed using a tem-
共3兲 plate formed with a thick-film photoresist 共SU-8兲. We used
Here, ␶ = ␳R2 / 8␩. The value of ␶ is in the order of PDMS not only because the microstructures are formed eas-
milliseconds16 and is negligible in our time scale. Since the ily and the technique is widely used but also because the
latter part of Eq. 共3兲 is x, Eq. 共3兲 becomes Eq. 共1兲 when t wettability of the surface can be changed in a wide range by
Ⰷ ␶. On the other hand, when t ⬇ 0, Eq. 共3兲 becomes an oxygen plasma treatment. The oxygen plasma treatment

冉 冊
was conducted using a Samco BP-1 basic plasma kit at an
2␥LV cos ␪ 1/2
RF power of 20 W and an oxygen flow rate of 20 ml/ min.
ẋ = . 共4兲
␳R The wettability was adjusted by changing the treatment time.
As is well known, the effect of the plasma oxidation is tem-
We then consider a capillary whose radius is changed to
porary, and the hydrophilic surface recovers to the initial
r from x = l and the displacement of the meniscus from the
hydrophobic surface as time elapses.19 Therefore, related ex-
edge of the region, z. If ż = 0 at t = 0 and z is small, the
periments were conducted immediately after the treatment.
following equation is obtained for ż;
The plasma-treated PDMS substrate adhered well to the
R2␥LV cos ␪ glass substrate by only exerting a slight pressure between the
ż = 兵1 − exp共− t/␶兲其. 共5兲
4r␩l two substrates.
For the characterization of the valve, the test device
As in Eq. 共3兲, ␶ is negligible. Therefore, Eq. 共5兲 again be- shown in Figs. 1共b兲 and 1共c兲 was fabricated. The valve action
comes the Washburn equation was based on direct electrowetting on a gold electrode.20 The
R2 basic structure consisted of a glass substrate with a three-
ż = ␥LV cos ␪ . 共6兲 electrode system to control electrowetting and a PDMS sub-
4r␩l
strate with an injection port, a microflow channel, and a
When ż ⫽ 0 at t = 0, the transient stage is also characterized valve structure. The length of the valve area along the flow
by ␶, and ż becomes Eq. 共6兲 immediately thereafter. channel was 500 ␮m. The electrode edge of the inlet side
In converting the equations for a rectangular flow chan- was located at 10 mm from the inlet of the flow channel. The
nel with height h and width w, R is replaced with hydraulic width of the flow channel was changed at the valve area to
radius RH, which is defined as13 control the movement of the transported solution. Metal lay-
ers were sputter-deposited, and chemical etching or a lift-off
RH = hw/共h + w兲. 共7兲
process was used for patterning. A base layer and the work-
Furthermore, a consideration of the change in the free energy ing electrodes for the valves were formed with a gold/
suggests that 2共h + w兲␥LV cos ␪ in the equation should further chromium layer. A Ag/ AgCl reference electrode and a plati-
[This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP:
131.187.254.4 On: Sat, 22 Nov 2014 22:11:04
034903-3 Satoh et al. J. Appl. Phys. 103, 034903 共2008兲

FIG. 1. Flow channel structures used for characterization. 共a兲 Flow channel formed with a glass substrate and a PDMS substrate. 共b兲 Flow channel with a
narrowed portion for a valve and electrodes used for operation. 共c兲 Magnified view of the valve area. 共d兲 Flow channels with a mixing valve. 共e兲 Magnified
view of the mixing area. 共f兲 Cross section of the mixing area and the flow channels. W.E., working electrode; R.E., reference electrode; and A.E., auxiliary
electrode.

num auxiliary electrode were formed in the injection port. A flow channel walls, was 15 deg. Unless otherwise noted, the
AgCl layer was grown on the silver pattern by applying PDMS flow channel was used without the oxygen plasma
1.0 ␮A for 1 min in a 1.0 M KCl–HCl solution 共pH 2.2兲. A treatment 共␪PDMS = 110 deg兲.
PDMS flow channel was formed as mentioned earlier. The
active areas of the electrodes were delineated with the PDMS
substrate, which also worked as an insulating layer. After the
flow channel structures and the electrodes were aligned, the
D. Experimental procedure
PDMS substrate was placed on the glass substrate and fixed.
Unless otherwise noted, the width and height of the flow A 1.0 M KCl solution was used as a test solution. The
channel used in the devices in Figs. 1共a兲–1共c兲 were 300 and static contact angle was measured with a droplet of 3 ␮l of
40 ␮m, respectively. To demonstrate the valve function in the solution using a Keyence VB-7010 charge coupled de-
complicated networks of flow channels, crossed, comb- vice 共CCD兲 camera and a VB-G25 multi-angle measurement
shaped, and tree-shaped flow channels with valves were also system. The movement of the solution in the flow channel
formed 共see Fig. 8兲. was recorded using the CCD camera. For this purpose, fluo-
Figures 1共d兲–1共f兲 show a test device used to mix two rescein 共1 mM兲 was added to visualize the liquid column.
solutions. A long rectangular gold working electrode was The flow velocity was calculated as an average at 10 mm
formed between two flow channels as a mixing valve. To from the inlet of the flow channel from the displacement of
effectively prevent two solutions from flowing into the other the meniscus and the time for the liquid column to reach 9.5
compartment, an array of rectangular PDMS micropillars and 10.5 mm. The theoretical values of the flow velocity
was formed at the mixing area. The area between the arrays refer to those at 10 mm. When necessary, the viscosity of the
of the micropillars formed the mixing area 关Figs. 1共e兲 and solution was adjusted by adding glycerol or BSA to the so-
1共f兲兴. The length, width, and height of the area were 5 mm, lution. The viscosity was measured using an Uberode-type
140 ␮m, and 70 ␮m, respectively. A Ag/ AgCl reference viscometer 共SU-5824, Sibata Scientific Technology, Tokyo,
electrode was formed at the end of one of the flow channels, Japan兲.
and the valve electrode was used in a two-electrode configu- To characterize the performance of the valve, a potential
ration. was applied to the gold working electrode with respect to the
Without the plasma treatment, the static contact angle on on-chip Ag/ AgCl electrode using a Hokuto-Denko HA151
PDMS 共␪PDMS兲 was 110 deg and could be decreased to potentiostat/galvanostat. Unless otherwise noted, the applied
10 deg by the plasma treatment. On the other hand, the con- potential was −0.9 V. All experiments were conducted at
tact angle of the glass substrate, which worked as one of the room temperature.
[This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP:
131.187.254.4 On: Sat, 22 Nov 2014 22:11:04
034903-4 Satoh et al. J. Appl. Phys. 103, 034903 共2008兲

21兲 and 0.98 mPa s, respectively. With the PDMS substrate


of a fixed contact angle, the flow velocity changes signifi-
cantly by changing the width of the flow channel when the
width is below 300 ␮m 关Fig. 2共a兲兴. However, the depen-
dence is weaker for flow channels wider than 300 ␮m. In
addition, the flow velocity increases monotonically as ␪PDMS
decreases. The calculated flow velocity becomes negative de-
pending on the values of the parameters. In this case, the
solution does not penetrate into the flow channel, and the
flow velocity should be zero. A similar tendency is observed
when the height of the flow channel is changed 关Fig. 2共b兲兴.
However, as seen in the curve at ␪PDMS = 120 deg, the flow
velocity decreases with the increase in the height depending
on the condition. Figure 2共c兲 shows the dependence of the
flow velocity on the reciprocal of the viscosity of the solu-
tion. A clear 1 / ␩ dependence of the flow velocity was ob-
served in the vicinity of the calculated straight line, indicat-
ing increasing difficulty in mobilizing a solution of a higher
viscosity.

B. Transport of fluid in flow channels


We then examined the dependence of the flow velocity
on ␪PDMS and the width of the flow channel experimentally
using the device shown in Fig. 1共a兲 关Fig. 3共a兲兴. The lines
indicate changes calculated using Eq. 共8兲. Overall, the ten-
dency of the experimental values was close to that antici-
pated from the Washburn equation. The flow velocity in-
creased as ␪PDMS decreased, and the width of the flow
channel increased. However, the discrepancy between the ex-
perimental and theoretical values at lower ␪PDMS values sug-
gests that the PDMS surface had become somewhat more
hydrophobic before the measurement started. In addition,
there may be a difference in the wettability between the in-
side of the flow channel and the surface on which we mea-
sured the contact angle due to the difference in microscopic
roughness. Figure 3共b兲 shows the dependence of the flow
velocity on the height of the flow channel. The flow velocity
increased as the height increased to 80 ␮m and leveled off
FIG. 2. Dependence of the theoretical flow velocity on the device param-
with higher flow channels, showing good agreement with the
eters. 共a兲 Dependence of the flow velocity on the width of the flow channel
and the contact angle on PDMS, ␪PDMS. h, 40 ␮m; ␪glass, 15 deg. The nu- theoretical values.
merals in the graph indicate the width of the flow channel. 共b兲 Dependence The dependence of the flow velocity on the viscosity of
of the flow velocity on the height of the flow channel and ␪PDMS. w, the solution was also examined by changing the viscosity of
300 ␮m; ␪glass, 15 deg. 共c兲 Dependence of the flow velocity on the recipro-
cal of the viscosity of the solution ␩ and ␪PDMS. h, 40 ␮m; w, 300 ␮m;
the solution with glycerol 关Fig. 3共c兲兴. The change in the con-
␪glass, 15 deg. In 共b兲 and 共c兲, the numerals in the graph indicate ␪PDMS. tact angle was negligible with glycerol of the maximum con-
centration. The measured values of the flow velocity agreed
well with Eq. 共8兲. We also conducted the same experiment
III. RESULTS AND DISCUSSION using BSA to change the viscosity. Although the slight adhe-
A. Theoretical model of a moving liquid column in a sion of BSA to the walls of PDMS and concurrent changes in
flow channel the property of the microfluidic system were anticipated, the
obtained values were close to those obtained with glycerol.
The time ␶ that characterizes the initial transient stage The result indicates that the influence of the single use of
becomes 0.16 ms when the width and height of the flow BSA solution is negligible, and the solution can also be
channel are 300 ␮m and 40 ␮m, respectively, which is transported like the glycerol solution.
shorter than the time required for the microfluidic transport
by several orders of magnitude. Therefore, the transient stage
C. Application to a valve structure to stop a moving
can actually be ignored in the following discussions.
liquid column
Figures 2共a兲 and 2共b兲 show the dependence of the theo-
retical flow velocity on the width and height of the flow The confirmation of the applicability of Eq. 共8兲
channel and ␪PDMS. Here, ␥LV and ␩ are 72.8 mN/ m 共Ref. prompted us to try to realize valves based on electrowetting.
[This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP:
131.187.254.4 On: Sat, 22 Nov 2014 22:11:04
034903-5 Satoh et al. J. Appl. Phys. 103, 034903 共2008兲

FIG. 4. 共Color online兲 Procedure for the valve action. 共a兲 A solution is
moving in the flow channel. 共b兲 The solution arrives at the edge of the valve
area under the off state. 共c兲 The solution moves on the valve area under the
on state. 共d兲 After the solution passes the valve area, it moves again in the
flow channel.

Figure 4 explains the valve action we tried to realize.


Initially, the potential is not applied to the valve’s working
electrode 共off state兲. When a solution is filled in the injection
port, it moves in the flow channel by capillary action 关Fig.
4共a兲兴. When the solution arrives at the valve area, the front of
the column slightly wets the electrode but stops there 关Fig.
4共b兲兴. When an appropriate potential is applied to the work-
ing electrode 共on state兲, the solution moves in the valve area
again 关Fig. 4共c兲兴. After the solution passes the valve area, it
moves again in the extending flow channel by capillary ac-
tion 关Fig. 4共d兲兴. The technique to stop a solution in a hydro-
phobic portion has been called a hydrophobic valve and has
been used in various forms.24–27 However, opening of previ-
ous hydrophobic valves has been carried out by applying air
pressure. On the other hand, our valve depends on changes in
the capillary force controlled by electrical signals. Therefore,
the integration of necessary components is easily achieved.
The effectiveness of the stopping function of the valve
shown in Figs. 1共b兲 and 1共c兲 was checked by changing ␪PDMS
and the width of the valve area. Figure 5 shows the move-
FIG. 3. Comparison between the theoretical and experimental flow veloci- ment of a fluorescein solution when ␪PDMS and the width of
ties. 共a兲 Dependence of the flow velocity on the contact angle on PDMS, the valve area were changed. When ␪PDMS was 110 deg, the
␪PDMS. Width of the flow channel: 䊊, 100 ␮m; 䊏, 300 ␮m; 䉭, 500 ␮m.
The curves in the graph show the change in the theoretical flow velocity. 共b兲
injected solution stopped with all the valve structures 关Figs.
Dependence of the flow velocity on the height of the flow channel. The 5共I兲–5共V兲兴. Gradation of the fluorescence image was ob-
curve shows the theoretical value. ␪PDMS, 110 deg 共no plasma treatment兲; served near the valve area. Although the arrival of the me-
␪glass, 15 deg, w, 300 ␮m. 共c兲 Dependence of the flow velocity on the recip- niscus at the edge of the electrode could be confirmed, the
rocal of the viscosity of the sample solution. 䊊, glycerol; 䊏, BSA. Five runs
were made for each experiment, and the averages and standard deviations
gradation of the image suggests that the solution reached the
are shown. ␪PDMS, 110 deg 共no plasma treatment兲; ␪glass, 15 deg; h, 40 ␮m; valve area only on the glass side. The extent of the intrusion
w, 300 ␮m. of the solution into the valve area depended on the dimen-
sions of the area. When the stopping was effective, the intru-
For this purpose, a gold working electrode was formed at the sion of the solution was negligible compared with the elec-
bottom of the flow channel 关Figs. 1共b兲 and 1共c兲兴. The sput- trode length. However, in some extreme cases, the solution
tered gold thin film was hydrophilic immediately after de- moved by approximately 20% of the electrode area. When
posited. However, after it was exposed to the atmosphere, it ␪PDMS was decreased to 100 deg, the solution passed the
rapidly became hydrophobic. The unavoidable phenomenon valve areas of 200, 500, and 1000 ␮m width without control
has been explained by the contamination by carbonaceous 关Figs. 5共III⬘兲–5共V⬘兲兴. Decreasing ␪PDMS further to 95 deg
compounds.22,23 In a finally stabilized state, all gold elec- made the situation even worse. In this case, none of the
trodes in all devices used for characterization showed the structures could suppress spontaneous passage of the solu-
same wettability reproducibly. Typically, the contact angle of tion 关Fig. 5共I⬙兲–5共V⬙兲兴.
a droplet of a 1.0 M KCl solution on the gold electrode was The stopping function can also be checked on the graph
72 deg without applying a potential. When −0.9 V was ap- shown in Fig. 6共a兲. Points that correspond to the structures
plied, it decreased to 25 deg. shown in Fig. 5 are also marked in the graph. The points on
[This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP:
131.187.254.4 On: Sat, 22 Nov 2014 22:11:04
034903-6 Satoh et al. J. Appl. Phys. 103, 034903 共2008兲

indicate that the solution passes the valve area. The results
with the structures in Fig. 5 and the position of the points in
Fig. 6共a兲 agree well. Namely, points corresponding to the
successful stopping of intrusion are on the abscissa, whereas
those corresponding to failed cases are on the curves.

D. Opening the valve by electrowetting


We then checked the movement of solution in the valve
area. The change in the wettability of the gold electrode at
the bottom of the area caused by electrowetting changes the
non-zero region of the curves. Figures 6共a兲 and 6共b兲 show the
graphs under the off state and on state, respectively. It is
noteworthy that the nonzero region of the curves is reduced
by applying the potential 关Fig. 6共b兲兴. As a result, all the
points, including those on the abscissa in Fig. 6共a兲, are on the
curves, indicating that the stopped liquid column can be mo-
bilized again. Figure 6共c兲 shows the movement of the solu-
tion through a valve that functioned as expected. The solu-
tion could be stopped under the off state and could be
FIG. 5. 共Color online兲 Movement of the solution in the valve area when the
width of the valve area and ␪PDMS were changed. ␪PDMS: 共I兲–共V兲, 110 deg;
mobilized again under the on state.
共I⬘兲 – 共V⬘兲, 100 deg; 共I⬙兲 – 共V⬙兲, 95 deg. Width of the valve areas: 共I兲, 共I⬘兲, To examine the effect of changing the wettability of the
共I⬙兲, 50 ␮m; 共II兲, 共II⬘兲, 共II⬙兲, 100 ␮m; 共III兲, 共III⬘兲, 共III⬙兲, 200 ␮m; 共IV兲, gold surface, the potential of the gold electrode was gradu-
共IV⬘兲, 共IV⬙兲, 500 ␮m; 共V兲, 共V⬘兲, 共V⬙兲, 1000 ␮m. ally changed from 0 V to the negative side, and the electrode
potential at which the meniscus began to move was mea-
the abscissa 共i.e., zero flow velocity兲 indicate that the solu- sured 共Fig. 7兲. In the flow channels of wider valve areas, a
tion can be stopped, whereas those on the nonzero curves potential of −0.6 V was enough to mobilize the meniscus.

FIG. 6. 共Color online兲 Dependence of the flow velocity on ␪PDMS and the width of the flow channel when ␪Au was 72 共a兲 and 25 deg 共b兲. 共I兲 – 共V⬙兲 correspond
to the cases in Fig. 5. The numerals near the curves indicate ␪PDMS. The inset shows the magnified view near the origin. The pictures in 共c兲 show the movement
of the fluorescein solution through the valve area. 共1兲 Solution stopped at the valve area under the off state. 共2兲 Solution moving on the valve area under the
on state. 共3兲 Solution moving in the flow channel.
[This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP:
131.187.254.4 On: Sat, 22 Nov 2014 22:11:04
034903-7 Satoh et al. J. Appl. Phys. 103, 034903 共2008兲

flow velocity in Figs. 6共a兲 and 6共b兲. The viscosity of the


solution changes the nonzero velocity overall. In other
words, the discussion above regarding the valve function
should apply irrespective of the viscosity of the solution,
although the velocity under the on state may become unac-
ceptably long with more viscous solutions.
The results presented in these experiments pose a prob-
lem of inconsistency. To stop a solution more effectively, the
walls of the valve area must be hydrophobic overall under
the off state. On the other hand, to increase the flow velocity
in the flow channel other than the valve area, the walls must
be sufficiently hydrophilic. To solve the problem, the wetta-
bility of the valve area and the flow channel area should
ideally be changed. The use of an air layer with the wide
valve compartment used in one of our devices may be such
an example.28
FIG. 7. Dependence of the threshold potential E to mobilize the liquid The simple structure of a hydrophilic flow channel with
column on the width of the valve area. Five runs were made for each ex- a valve is applicable to the construction of networks of
periment, and the averages and standard deviations are shown. ␪PDMS,
branched flow channels that can handle many solutions 共Fig.
110 deg 共no plasma treatment兲. The inset shows the dependence of the con-
tact angle of a droplet of a 1.0 M KCl solution on a gold electrode ␪Au on 8兲. In each device shown in the figure, a solution was first
the applied potential. The reference electrode is a thin-film Ag/ AgCl elec- filled in the injection port on the left. The solutions moved
trode directly exposed to the solution. spontaneously and immediately to the first valves. When the
valve electrodes at the inlet of desired flow channels were
However, with narrower valve areas, the threshold potential switched on, the solution passed the valve areas and was
shifted to the negative side, suggesting that a stronger motive transported in the flow channels. By repeating the same pro-
force was required. When the width of the flow channel and cedure, the solutions in the other flow channels could be
the length and width of the valve area were 300, 500, and mobilized.
50 ␮m, respectively, and ␪Au = 25 deg, the time for the me- In this system, the potential was applied to the valve
niscus to pass the valve area was calculated to be 1.0 s. The working electrode only during the passage of the solution. As
experimental values obtained from five experiments distrib- a result, the measured power consumption was less than
uted between 1.3 and 2.3 s. The discrepancy seems to derive 10 ␮W even in the highest case. Along with the switching
from the microscopic roughness on the PDMS walls, which speed, the power consumption could be reduced further by
is actually recognized under a microscope with high magni- designing a shorter valve electrode.
fication. As reported earlier, the contact angle in the Washburn
The geometry of the flow channel and the wettability of equation should be the dynamic contact angle. However,
the flow channel walls determine the boundary at the zero measuring the dynamic contact angle that depends on the

FIG. 8. 共Color online兲 Microfluidic transport of a fluorescein solution in a crossed network 共a兲, a comb-shaped network 共b兲, and a tree-shaped network 共c兲 of
flow channels. The arrows indicate the movement of the solution from opened valves. The position of the valves is indicated in the figures. w⬘, 150 ␮m; w,
300 ␮m; h, 40 ␮m.
[This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP:
131.187.254.4 On: Sat, 22 Nov 2014 22:11:04
034903-8 Satoh et al. J. Appl. Phys. 103, 034903 共2008兲

position of the flow channel for designing the valve system is


unrealistic. The dynamic contact angle depends on the cap-
illary number Ca= ␩ẋ / ␥LV. As a general tendency, the differ-
ence between the dynamic and static contact angles de-
creases with the decrease in Ca, and the dynamic contact
angle becomes more independent of Ca in the lower region
of Ca with the increase in the static contact angle. In the case
of our system, Ca was on the order of 10−4 – 10−3. Previous
results suggest that the dynamic contact angle can be ap-
proximated well with the static contact angle in the range of
Ca.29 In fact, the data presented in Figs. 3 and 6 show an
excellent agreement between the theoretical and experimen-
tal values. In other words, the static contact angle could be
used at least for designing systems with the same combina-
tion of materials and dimensions without accompanying sig-
nificant errors.

E. Application to a mixing valve


FIG. 9. 共Color online兲 Mixing of solutions using the mixing valve. 共a兲
The valves can also be used for the mixing of two solu- Mixing area showing fluorescein solutions filled in two flow channels on
tions. Various geometries and sizes will be considered for a both sides of the valve. 共b兲 and 共c兲 show the magnified view of the mixing
area. 共b兲 Before mixing. 共c兲 After mixing.
mixing valve, and the single valve structures discussed up to
now may be used in many cases. However, as a relatively
difficult case, mixing of solutions between two parallel flow flow channel, a moving liquid column can be stopped or
channels is considered here. To this end, the long valve struc- passed at the valve area as intended. Complicated networks
ture shown in Figs. 1共d兲–1共f兲 placed between the two flow of flow channels that transport solutions to desired directions
channels would facilitate rapid mixing. However, as is evi- can be realized. The valve can also be used for the mixing of
dent from the previous discussions, the control of the move- solutions. Since the movement of the liquid column in the
ment of a solution in a long valve area becomes difficult. flow channel is spontaneous and a potential is applied to the
Indeed, with only the long mixing electrode, the two solu- valve working electrode only for a short time during the
tions penetrated into the valve area in an uncontrollable man- passage of the solution, power consumption can be mini-
ner and were mixed before the potential was applied. mized. Although our device was based on direct electrowet-
To stop the solutions as intended, the previous discus- ting on a gold electrode, the same direction for valve design-
sions provide a solution. We formed PDMS micropillars to ing applies to the case of electrowetting on dielectric. A
segment the long valve area 关Fig. 1共e兲兴. The pillars were convincing advantage of our device is its simplicity. It can be
rectangles of 100⫻ 80 ␮m2, and the interpillar distance a basic building block to construct a highly integrated micro-
共edge to edge兲 was 100 ␮m. When the two solutions were fluidic system that is capable of handling liquids in compli-
introduced to the end of the flow channels, the pillars could cated situations.
effectively block the intrusion of the solutions under the off
state 关Figs. 9共a兲 and 9共b兲兴. Furthermore, when the potential ACKNOWLEDGMENTS
was applied to the mixing electrode, the stopped solutions This study was supported by Grants-in-Aid for Scientific
could be mixed 关Fig. 9共c兲兴. It is noteworthy that the reference Research on Priority Areas and by the 21st Century COE
electrode is connected to only one of the flow channels. Program, both of which are under the Ministry of Education,
Therefore, the solution in the flow channel with the reference Culture, Sports, Science, and Technology, Japan.
electrode started moving first and mixed with the solution on
the other side. A point which needs further consideration is 1
H. Suzuki and R. Yoneyama, Sens. Actuators B 96, 38 共2003兲.
2
the unnegligible dead volume of the valve area, which affects W. Satoh, H. Hosono, and H. Suzuki, Anal. Chem. 77, 6857 共2005兲.
3
the mixing ratio as the solution volume decreases. To cope C. Quilliet and B. Berge, Curr. Opin. Colloid Interface Sci. 6, 34 共2001兲.
4
J.-Y. Cheng and L.-C. Hsiung, Biomed. Microdevices 6, 341 共2004兲.
with this problem, the electrode should be narrowed to a 5
K. Morimoto and H. Suzuki, Biosens. Bioelectron. 22, 86 共2006兲.
limit considering the interpillar distance. 6
L. Tanguy, T. Leïchlé, and L. Nicu, J. Appl. Phys. 101, 044907 共2007兲.
7
J.-C. Baret, M. Decré, S. Herminghaus, and R. Seemann, Langmuir 21,
12218 共2005兲.
IV. CONCLUSIONS 8
J.-C. Baret, M. M. J. Decré, S. Herminghaus, and R. Seemann, Langmuir
A microfluidic system based on capillary action and 23, 5200 共2007兲.
9
E. W. Washburn, Phys. Rev. 17, 273 共1921兲.
electrowetting can be designed on the basis of the Washburn 10
C. H. Bosanquet, Philos. Mag. 45, 525 共1923兲.
11
equation. The flow velocity in a microflow channel can be J. Szekely, A. W. Neumann, and Y. K. Chuang, J. Colloid Interface Sci.
controlled by changing the wettabillity of the channel walls 35, 273 共1971兲.
12
A. Marmur, J. Colloid Interface Sci. 122, 209 共1988兲.
and the geometry of the flow channel. A gold valve electrode 13
E. Delamarche, A. Bernard, H. Schmid, A. Bietsch, B. Michel, and H.
facilitates the control of microfluidic transport. By properly Biebuyck, J. Am. Chem. Soc. 120, 500 共1998兲.
14
designing the valve structure, particularly, the width of the S. Levine and G. H. Neale, J. Chem. Soc., Faraday Trans. 2, 71, 12 共1975兲.
[This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP:
131.187.254.4 On: Sat, 22 Nov 2014 22:11:04
034903-9 Satoh et al. J. Appl. Phys. 103, 034903 共2008兲

15 23
B. V. Zhmud, F. Tiberg, and K. Hallstensson, J. Colloid Interface Sci. 228, T. Smith, J. Colloid Interface Sci. 75, 51 共1980兲.
263 共2000兲. 24
M. A. Burns, B. N. Johnson, S. N. Brahmasandra, K. Handique, J. R.
16
D. Quéré, Europhys. Lett. 39, 533 共1997兲. Webster, M. Krishnan, T. S. Sammarco, P. M. Man, D. Jones, D.
17
A. Janshoff and S. Künneke, Eur. Biophys. J. 29, 549 共2000兲. Heldsinger, C. H. Mastrangelo, and D. A. Burke, Science 282, 484 共1998兲.
18
E. Kim, Y. Xia, and G. M. Whitesides, Nature 共London兲 376, 581 共1995兲. 25
K. Hosokawa, T. Fujii, and I. Endo, Anal. Chem. 71, 4781 共1999兲.
19
H. Hillborg, J. F. Ankner, U. W. Gedde, G. D. Smith, H. K. Yasuda, and K. 26
K. Handique, D. T. Burke, C. H. Mastrangelo, and M. A. Burns, Anal.
Wikström, Polymer 41, 6851 共2000兲.
20 Chem. 72, 4100 共2000兲.
J. Lee, H. Moon, J. Fowler, T. Schoellhammer, and C.-J. Kim, Sens. 27
Actuators, A 95, 259 共2002兲. M. Yamada and M. Seki, Anal. Chem. 76, 895 共2004兲.
28
21
D. Myers, Surfaces, Interfaces, and Colloids, 2nd ed. 共Wiley-VCH, New N. Nashida, W. Satoh, J. Fukuda, and H. Suzuki, Biosens. Bioelectron. 22,
York, 1999兲. 3167 共2007兲.
22 29
N. K. Adam, The Physics and Chemistry of Surfaces, 3rd ed. 共Oxford K. Ishimi, J. Mohri, H. Mukouyama, and H. Ishikawa, J. Chem. Eng. Jpn.
University Press, London, 1941兲. 31, 914 共1998兲.

[This article is copyrighted as indicated in the article. Reuse of AIP content is subject to the terms at: http://scitation.aip.org/termsconditions. Downloaded to ] IP:
131.187.254.4 On: Sat, 22 Nov 2014 22:11:04

You might also like