Engineering, 2009, 2, 111-116
doi:10.4236/eng.2009.12013 Published Online August 2009 (http://www.SciRP.org/journal/eng/).
Copyright © 2009 SciRes. ENGINEERING
Fabrication of Si-PDMS Low Voltage Capillary
Electrophoresis Chip
Wenwen GU1,2,3,4, Zhiyu WEN1,2,3,4, Zhongquan WEN1,2,3,4, Yi XU1,2,3,
Fengfei LIANG1,2,3, Xiaoguo HU1,2,3
1Key Laboratory of Fundamental Science of Micro/Nano-Device and System Technology, Chongqing, China
2National Center for International Research of Micro/Nano-System and New Material Technology, Chongqing, China
3Microsystem Research Center, Chongqing University, Chongqing, China
4College of Optoelectronic Engineering, Chongqing University, Chongqing, China
Received May 11, 2009; revised July 2, 2009; accepted July 10, 2009
ABSTRACT
This paper discusses the fabrication of Si-PDMS low voltage capillary electrophoresis chip (CE chip). Ar-
rayed-electrode which is used to apply low separation voltage is fabricated along the sidewalls of the separa-
tion channel on the silicon based bottom part. Isolation trenches, which are placed surrounding the ar-
rayed-electrode, insure the insulation between the arrayed-electrode, as well as arrayed-electrode and liquid
in the micro channel. Polydimethylsilicone (PDMS) is used as the cover. PDMS and silicon based bottom
part are reversible sealed to attain Si-PDMS low voltage CE chip. Experiments have been done to obtain op-
timum electrophoresis separation condition: separation voltage is 45V, switch time is 2s and the Phe and Lys
electrophoresis separation is successful.
Keywords: Low Voltage, Arrayed-Electrode, Si-PDMS, CE Chip
1. Introduction
Lab on a Chip, or called Miniaturized Total Analysis
System (µ-TAS [1]), which has features of miniature,
fast, high performance and throughput, has become a hot
research topic in analytical chemistry. Capillary Elec-
trophoresis Chip (CE chip) is a highly integrated minia-
ture separation and analysis device within the develop-
ment of biotechnology and MEMS (Micro-Electro-Mechanic
Systems) technology. It can integrate sample treatment,
injection, separation and detector into a microchip which
is only several square centimeters. In CE chip, micro
channels form network, and controlled microfluidic runs
through all the system [2]. With the development of CE
chip and widely applications, many fields such as disease
diagnosis, environmentent monitoring, new drug devel-
opment, food safety inspection will be changed thor-
oughly. Nowadays, it has already become one of the
most important study subjects in chemistry, life science,
MEMS, physics, micro-electronics and etc [3,4].
Taking a wide view of the related research status [5-8],
working voltage which is from several hundreds to thou-
sands is directly applied in the two ends of the separation
channel of the CE chip. There are some shortages bought
by high voltage, such as huge equipments, high thermal
effect and high safety protection requirements for labo-
ratory operators. High voltage also restricts the minia-
turization, home application and portability for CE chip.
According to the moving gradient electrical field the-
ory of CE chip, the separation channel can be equivalent
to series connections of several shorter ones. Using ar-
rayed-electrode to apply low separation voltage section
by section can obtain the demanded high separation elec-
tric field. So the difficult problem brought by CE chip
requiring high separation voltage has been overcome
[9-12].
Based on the idea above, a new approach has been
proposed to fabricate low voltage CE chip. Silicon-on-
insulator (SOI) wafer is used as the substrate material of
the silicon based bottom part, where there is a cross
channel and arrayed-electrode. Arrayed-electrode and
isolation trenches are fabricated along the micro channel
W. W. GU ET AL
Copyright © 2009 SciRes. ENGINEERING
112
sidewalls. The arrayed-electrode is used to apply low
separation voltage. The isolation trenches insure the in-
sulation between the arrayed-electrode, as well as ar-
rayed-electrode and liquid in the micro channel. PDMS
(Polydimethylsilicone) is used as the cover of the CE
chip. The low voltage CE chip is obtained by reversible
sealing the silicon based bottom part and the PDMS
cover.
2. Low Voltage Separation Principle
The length of separation channel for conventional CE
chip is several centimeters, and tens of kilovolts voltage
must be applied in two ends of the separation channel.
According to the principle of electrophoresis separation
and the requirement of invariable electric field intensity
in the separation channel, we proposed a thought of ap-
plying voltage section by section and circularly in the
separation channel. Therefore, we design and fabricate
arrayed-electrode with equal interval in the micro chan-
nel and periphery controlling circuit to control the time
and range of the voltage on the arrayed-electrode. Figure
1(a) shows the model of low voltage separation. During
the electrophoresis separation process, voltage is firstly
applied on the first and third arrayed-electrode to drive
sample move for a period time T (we call it switch time).
Then, voltage is applied on the second and forth ar-
rayed-electrode for the same switch time. Next, voltage
is applied on the rest of the arrayed-electrode which is
followed this rule until the final pair of arrayed-electrode
is affected. After the first cycle is finished, it goes to the
next cycle. Voltage begins to apply on the first and third
arrayed-electrode again. From Figure 1(a), it is obvious
that the method for applying voltage is totally depended
on the switch time and voltage applied on the ar-
rayed-electrode. Therefore, we can select and optimize
the separation condition to obtain the best result.
Figure 1(b) shows the control system for low voltage
separation. The main electronic components are Micro-
programmed Control Unit (MCU), communication in-
terface, current amplifier circuit and array relay. Com-
puter sends orders to MCU, which controls time se-
quence of voltage applied to every arrayed-electrode.
MCU is used to control array-relay to carry out one of
the three states of ground, high level or suspending on
the arrayed-electrode. After the electrophoresis separa-
tion is finished, the experiment results will return to
MCU, and be displayed in monitor screen.
3. Fabrication Process
3.1. Layout Design
Based on the electric and flow field simulating results of
Figure 1 Schematic diagram of low voltage separation (a)
model of low voltage separation; (b) control system.
Figure 2. Structure diagram of the low voltage CE chip.
low voltage CE chip [13,14], the structure of the CE chip
has been designed, and the geometry parameters have
been determined. The low voltage CE chip contains two
parts: one is the silicon based bottom part where there is
a cross microchannel and arrayed-electrode, and the
other is PDMS cover where there are four reservoirs. The
size of the designed CE chip is 3.9cm×1.7cm, where the
separation channel is 3cm in length, 80μm in width, and
15μm in depth and the injection channel is 6mm in
length, 40μm in width, 15μm in depth. Along the side-
walls of the injection and separation channel, there are
respectively 8 and 39 pairs of arrayed-electrode between
which the interval is 700μm. The specific dimensions of
the low voltage CE chip are showed in Figure 2.
W. W. GU ET AL
Copyright © 2009 SciRes. ENGINEERING
113
3.2. Silicon Based Bottom Part of Low Voltage
CE Chip
How to fabricate arrayed-electrode is the key point of
successful electrophoresis for low voltage CE chip. Be-
sides, how to insulate voltage and current between ar-
rayed-electrode is also very important. This paper pro-
poses using narrow channel deep trough etching [15] and
polysilicon refilling, so arrayed-electrode can be insu-
lated to isolated islands completely [16]. Then, arrayed-
electrode is formed by ions diffusion. We select SOI
(Silicon on Insulation) wafer as the substrate of the low
voltage CE chip, because the influence to device layer
caused by substrate (block effect) is reduced, as well as
the parasitic effect caused by silicon device. Figure 3
shows processing scheme of silicon based bottom part of
low voltage CE chip on SOI substrate.
1) Oxidize on the SOI wafer (device layer 15μm) to
form a SiO2 shielding layer with the thickness of
400-600nm as the insulating layer of the bottom of micro
arrayed-electrode; 2) Photoetch isolation regions to insu-
late arrayed-electrode; 3) Use Inductively Coupled Plas-
ma (ICP) to etch silicon in the isolation trenches with the
depth of 15μm; 4) Do isolation trenches cleaning: a) Use
glacial acetic acid and water (1:5) to deal with the isola-
tion trenches; b) Do normal RCA cleaning (1# NH4OH:
H2O2: H2O=1:2:7; 2# HCI: H2O2: H2O=1:2:7); c) Do
ultrasonic cleaning by deionized water; 5) Oxidize in the
isolation trenches to form a SiO2 insulating layer with the
thickness of 1000nm; 6) Use polysilicon to refill isola-
tion trenches with the thickness of 2μm; The optimum
conditions are as follows: polysilicon deposit is con-
trolled at 715-815nm/min, and temperature is 590-610
Degree Centigrade; 7) Oxidize to form a layer of SiO2; 8)
Photoetch the region of arrayed-electrode; 9) Boron ions
diffuse to form P+ arrayed-electrode with the junction
depth of 8-12μm; 10) Thermal oxidize to form a SiO2
shielding layer with the thickness of 6000
; 11) Pho-
toetch wire holes and sputter Al with the thickness of
1.2μm to lead out arrayed-electrode; 12) Alloy to form
ohmic contacts; 13) Use Plasma Enhance Chemical Va-
por Deposition (PECVD) to deposit a passivation layer
with the thickness of 1.2μm; 14) Photoetch bonding
points and etch SiO2; (14) Use Inductivity Coupled
Plasma (ICP) to etch silicon with the thickness of 15μm
until the layer of SiO2 of the SOI wafer is exposed.
3.3. Fabrication PDMS Cover
PDMS has some advantages, such as low surface free
energy (21.6dyn/cm), stable chemical properties. There
are also some features of flexible, good elasticity and
close contact with the silicon substrate. So PDMS is se-
lected as the cover of low voltage CE chip.
During the fabrication, firstly, PDMS monomer and
firming agent are mixed by the volume ratio of 10:1. Stir
uniformly, and pour it into a flat glass container. Then
Figure 3. Processing scheme of low voltage CE chip on SOI.
W. W. GU ET AL
Copyright © 2009 SciRes. ENGINEERING
114
pour prepolymer with the thickness of 3-5mm on it.
Secondly, put the container in the vacuum desiccator to
pump for 40 minutes until the air bubbles mixed in it are
completely removed. Thirdly, remove the container to a
baking oven and then solidify it for 4 hours in the condi-
tion of 60 Degree Centigrade. Finally, peel off PDMS
lightly from the glass container. Four holes each of
which has the diameter of 3mm are drilled in the corre-
sponding positions of PDMS as the reservoir. The func-
tion for them is to storage sample and waste.
3.4. Bond and Package
Because of good adhesiveness of PDMS, it can achieve
reversible and irreversible sealing with silicon material.
In order to do convenient and completely cleaning, we
make reversible sealing with PDMS cover and silicon
based bottom part. The specific operation steps are as
follows: immerge PDMS cover and silicon based bottom
part in the ethanol and distilled water, evaporate to dry
ness by nitrogen and then put them together. It is impor-
tant to align the two parts. The self-fabricated Si-PDMS
low voltage CE chip has good compatibility at
the Si-PDMS interface, no leakage, no deformation,
good stability and well sealing in the routine operation
condition.
Because the number of bond contact in the low voltage
CE chip is far more than that of pins in general cellpack
ing, we design PCB to package the self-fabricated low
voltage CE chip. The size of the PCB is 4.43cm×
3.38cm, and the pads are laid on it to bond with bond
contact in low voltage CE chip by Si-Al-wire. Figure 4
shows the photo of Si-PDMS low voltage CE chip with
PCB packaging.
4. Results and Discuss
4.1. Inspection of the Fabricated Structure
The fabricated low voltage CE chip is tested by mor-
phology generation and detection system module of
MEMS measurement and micro operation system (Robot
Research Institute of Harbin Institute of Technology,
Figure 4. Si-PDMS low voltage CE chip with PCB pacage.
Figure 5. SEM of micro-channel with array-electrodes.
Figure 6. 3-D generation graph of the microchannel.
China). Figure 5 shows the arrayed-electrode at the cross
channel. The measured values for width of the separation
and injection channel are 83μm and 42μm, where the
relative error is 3.61% and 4.76% respectively. Figure 6
shows the three-dimensional graph of the separation
channel. The measured depth value is 15μm, which is
consistent with our designed value.
4.2. Electrical Performance Test for Arrayed-Electrode
In order to test the electrical performance of the fabri-
cated low voltage CE chip, we test and measure the re-
sistance and breakdown voltage of the arrayed-electrode
to estimate the insulation and resistance breakdown. We
do ergodic experiment on all the arrayed-electrode to
measure the resistance of adjacent arrayed-electrode (re-
sistance for arrayed-electrode on 1st and 2nd, 2nd and
3rd, 3rd and 4th …until 38th and 39th). The value is in-
finite for each tested arrayed-electrode pair. It means the
isolation trenches are effective, and the insulation be-
tween the arrayed-electrode is achieved.
Semiconductor transistor testing instrument is used to
test the breakdown voltage of the fabricated low voltage
CE chip. We apply testing voltage on the adjacent ar-
rayed-electrode and test all the breakdown voltage on
arrayed-electrode (1st and 2nd, 2nd and 3rd, 3rd and
4th …until 38th and 39th). The average of the value is
W. W. GU ET AL
Copyright © 2009 SciRes. ENGINEERING
115
0
0.05
0.1
0.15
0.2
0123456789
t/min
u/mv
306V, and the standard deviation is 3.41V. Because the
voltage for low voltage electrophoresis separation is only
40-80V, the breakdown voltage satisfies our needs.
4.3 Low Voltage Electrophoresis Separation
4.3.1. Reagents
Fluorescein isothiocyanate (FITC) is obtained from Si-
nopharm Group Chemical Reagent Co. Ltd. (Shanghai,
China). Phenylalanine (Phe) and lysine (Lys) are pur-
chased from Shanghai Bio Life Science & Technology
Co. Ltd. (Shanghai, China). 2-(N-Morpholino) ethane-
sulfonic acid (MES) was obtained from AMRES Co.,
Hong Kong. All kinds of buffer solutions including MES,
His and borate are prepared with redistilled water in
0.1mol/L and diluted in suitable concentration prior to
use. All amino acids and stock sample solutions of FITC
are prepared respectively in redistilled water to a con-
centration of 10mmol/L. Then 10μL FITC solution and
10μL amino acid solutions are mixed and reacted for 12
hours in 25 Degree Centigrade. All the solutions are fil-
tered by 0.2μm filter membrane before being injected
into the low voltage CE chip.
4.3.2. Optimization of Experimental Conditions
During the electrophoresis separation, separation voltage
directly affects the peak time and efficiency of the sam-
ple. When the separation voltage is less than 30V (that is
to say, the field intensity is less than 200V/cm) the driv-
ing force will be too small; while when the separation
voltage is greater than 50V, there is Joule heat effect in
the CE chip. Experiment results show that the higher the
separation voltage is, the shorter the peak time is. How-
ever, if the separation voltage is too high, the peak will
come too quickly, and it is disadvantage for sample
separation; while the separation voltage is too small, the
peak will come too late, and it will lead to long analysis
time and worse the analysis efficiency. Finally, we chose
45V as the optimization working voltage for low voltage
electrophoresis separation.
Switch time is another factor which influences the
separation efficiency. If the switch time is too short,
movement velocity of sample can not catch up with the
velocity of switch time, so the zone of the sample is
likely to be cut off into several parts, and cause the base-
line turbulence. If switch time is too long, the zone of the
sample will accumulate. 2s is the optimal switch time for
low voltage electrophoresis separation when the separa-
tion voltage is 45V.
4.3.3. Low Voltage CE Chip Electrophoresis Separation
Phe and Lys electrophoresis separation experiments are
done in the optimal condition: separation voltage: 45V
(300V/cm); switch time: 2s. Figure 7 shows electropho-
resis spectrum of 10-4mol/L Phe and Lys. The peak time
Figure 7. Electrophoresis spectrum of of 10-4mol/L Phe and
Lys for low voltage CE chip.
for Phe is 6 minuets, while the peak time for Lys is 4
minuets, and the degree of separation is 2.0. From Figure
8, we got that the self-fabricated CE chip can analysis
and test biochemical sample through low voltage elec-
trophoresis separation, It reduces the separation voltage
which is thousands of volts to only tens of volts. During
the experiments, because the injection volume and time
is hard to control, the reproducibility of the testing re-
sults is not very good. In future work, we have to im-
prove and enhance the experimental technique.
5. Conclusions
We have fabricated a Si-PDMS low voltage CE chip. It
contains two parts: one is the silicon based bottom part
where there is a cross microchannel and arayed-electrode,
and the other is PDMS cover where there are four reser-
voirs to storage sample and waste. Arrayed-electrode
which is used to apply separation voltage is fabricated
along the micro channel sidewalls on the SOI wafer. In
order to insure the insulation between the ar-
rayed-electrode, isolation trenches are also fabricated.
PDMS and silicon based bottom part are reversible
sealed to attain Si-PDMS low voltage CE chip. Because
arrayed-electrode is the key point of successful electro-
phoresis of low voltage CE chip, the electrical perform-
ance of the arrayed-electrode has been tested, including
insulation and resistance breakdown. Results show the
resistance between arrayed-electrode is infinite and the
average of breakdown voltage is 306V. Electrophoresis
separation experiments have been done to obtain opti-
mum low voltage separation condition: separation volt-
age is 45V, the switch time is 2s and the Phe and Lys
electrophoresis separation is successful.
6. Acknowledgements
This research work was supported by Chinese National
Science and Technology Committee ‘863 Plan’
(2006AA04Z354) and ‘International Cooperation Plan’
(2006DFA13510).
W. W. GU ET AL
Copyright © 2009 SciRes. ENGINEERING
116
7. References
[1] A. Manz, N. Graber, and H. M. Widmer, “Miniaturized
total chemical analysis systems: A novel concept for
chemical sensing,” Sensors and Actuators B, Vol. 7, pp.
244-248, 1990.
[2] N. A. Lacher, K. E. Garrison, and R. S. Martin, “Micro-
chip capillary electrophoresis/electro-chemistry,” Elec-
trophoresis, Vol. 22, pp. 2526-2536, 2001.
[3] Y. Jin, G. A. Luo, and R. J. Wang, “Development of in-
tegrated capillary electrophoresis chips,” Chinese Journal
of Chromatography, Vol. 4, pp. 313-317, 2000.
[4] C. Koppmu and A. D. Manz, “Development in technol-
ogy and application of microsystems,” Current Opinion
in Chemical Biology, Vol. 1, pp. 410-419, 1997.
[5] J. C. Fister, S. C. Jacobson, and J. M. Ramsey, “Ultrasen-
sitive crosscorrelation electrophoresis on microchip de-
vices, Analytical Chemistry, Vol. 71, pp. 4460-4464,
1999.
[6] J. Qian, Y. Wu, H. Yang, A. C. Michael, “An integrated
decoupler for capillary electrophoresis with electrochemi-
cal detection: Application to analysis of brain microdialy-
sate,” Analytical Chemistry, Vol. 71, pp. 4486-4492,
1999.
[7] Y. Shi, P. C. Simpon, J. R. Scherer, and D. Wexler, “Ra-
dial capillary array electrophoresis microplate and scan-
ner for high-performance nucleic acid analysis,” Analyti-
cal Chemistry, Vol. 71, pp. 5354-5361, 1999.
[8] J. Wang, M. P. Chatrathi, B. Tian, and R. Polsky, “Micro-
fabricated electrophoresis chips for simultaneous bioas-
says of glucose, uric acid, ascorbic acid, and acetamino-
phen,” Analytical Chemistry, Vol. 72, pp. 2514-2518, 2000.
[9] Y. C. Lin and W. D. Wu, “Arrayed-electrode design for
moving electric field driven capillary electrophoresis
chips,” Sensors and Actuators B, Vol. 73, pp. 54-62,
2001.
[10] L. M. Fu and R. J. Yang, “Low-voltage driven control in
electrophoresis microchips by traveling electric field,”
Electrophoresis, Vol. 24, pp. 1253-1260, 2003.
[11] X. Li, Z. Y. Wen, and H. X. Li, “Low voltage separation
model and its control system for electrophoresis chip,”
Micronanoelectronic Technology, Vol. 7/8, pp. 344-346,
2003.
[12] Y. Wu, Z. Y. Wen, and Z. P. Jiang, “Low voltage separa-
tion model and discussion for electrophoresis chip,”
Opto-Electronic Engineering, Vol. 29, pp. 27-33, 2002.
[13] Z. Y. Wen, Y. Xu, and X. Li, “Electric field simulation of
separation mode on low voltage electrophoresis chip,”
Optoelectronic Engineering, Vol. 9, pp. 35-41, 2006.
[14] Y. Xu, Z. Y. Wen, and X. Li, “Fluidic field simulation of
separation mode on low voltage electrophoresis chip by
ConventerWare,” Chinese Journal of Sensors and Actua-
tors, Vol. 8, pp. 1070-1075, 2007.
[15] Z. Y. Zhang, S. L. Xu, and Y. K. Liu, “A Study on silicon
deep etching technology,” Microelectronics, Vol. 2, pp.
519-521, 2004.
[16] Y. Wu, Y. Q. Jiang, and Z. Y. Wen, “Development of
polycrystalline silicon micro-electrode array on silicon
substrate,” Semiconductor Optoelectronics, Vol. 4, pp.
317-319, 2005.