ISTP-16, 2005, PRAGUE 16

TH
INTERNATIONAL SYMPOSIUM ON TRANSPORT PHENOMENA
1
Abstract
The object of this research is to investigate
processes for fabricating micro-channels on
silicon wafers based upon TMAH wet-etching
approach. Effects of several etching fluid
options on various etching stoppers, etching
rates, and etched surface roughness are studied.
Experimental results showed that 5%wt TMAH
etching solutions with added 3g/L ammonium
peroxodisulfate (AP) and 14g/L silicon power
recipes can be adopted to fabricate optimal
micro-channels with 1.024 m/min etching rate
and 45.5 nm average etched-surface roughness
(Ra).
1 Introduction
Anisotropic silicon etching is a commonly
adopted technology to fabricate micro-
electromechanical structures (MEMS). Among
the etching fluid options, potassium hydroxide
(KOH), tetraethyl ammonium hydroxide
(TMAH) and ethylenediamine-pyrocatechol
(EDP) are three of the etching solutions usually
employed. Each of the three demonstrates
certain etching rates for certain materials and
stopped by corresponding etching barriers.
Since TMAH etching solution doesnt contain
toxic constitutions as EDP does and does hold
better selectivity for etching barriers, it has been
broadly utilized in the CMOS industry for
fabricating VLSI microelectronic circuits [1-3].
During last ten years, MEMS technology has
been strongly promoted to realize micro-sensors
as well as micro-actuators for next generation
applications, and typical usages include bio-
chips for medical industry as well as fuel-cells
for energy industry. It is known major
structures for these micro-devices must be
constructed based upon micro-channels and
micro-chambers, and fluid transportations,
mixings, or separations can therefore conducted
within the fabricated micro-structures. Hence,
TMAH wet-etching solution finds another usage
for MEMS applications in addition to VLSI
fabrications.
Main reason to adopt TMAH wet-etching
approach in this research as to construct fluid
micro-passages is based upon its low cost
feature and selective etching barrier aluminum.
However, TMAH solution still etches aluminum
in certain minor degree [4-9], and additions of
silicon-oxide or dissolutions of silicon powders
can decrease the pH value of the TMAH
solution [10] as to protect designated aluminum
area.
Hence, during this study the TMAH wet-etching
approach is implemented to fabricate micro-
channels on silicon wafers, and these micro-
passages are hereafter used to transport bio-
fluids once coupled to certain micro
electromechanical pumps, which are developed
in another corresponding research. As a result,
this paper presents a novel TMAH recipe
specifically for fabricating micro-channels.
Physical vapor deposition (PVD) method is also
employed to deposit aluminum layer on the
silicon wafers. The THAH fabrication process
features high etching rate for developing the
micro-structures within silicon matrix, and the
aluminum barriers are not attacked. Highly
smoothed micro-channel etched-surfaces on
silicon structures are obtained.

MICRO-CHANNEL FABRICATIONS WITH
TMAH ANISOTROPIC WET-ETCHING

Fu-Shin Lee*, Chih-Hsiung Chen*, Chiang-Chao Liao*, and Jyh-Ling Lin**
*Mechatronical Engineering Dept., Huafan University, Taipei, Taiwan (ROC)
**Electronics Engineering Dept., Huafan University, Taipei, Taiwan (ROC)
Corresponding author: fslee@huafan.hfu.edu.tw, (886)-(2)-2663-2102 ext.4016

Keywords: micro-channel, TMAH, surface roughness, biochip.
Fu-Shin Lee, Chih-Hsiung Chen, Chiang-Chao Liao, Jyh-Ling Lin
2
2. Design Stage for Micro-Channel Geometry
Geometry of the micro-channels,
preparation processes for TMAH etching
solutions, photomask design for micro-channels,
selections of process operation parameters, and
etching barrier layers preparations are explained
in the following.
The patterns of photomasks are designed using a
tool of a MEMS design software (L-EDIT of
MEMSPRO), and total length of the micro-
channels is 15000 m with a width of
2000 m. The patterns are converted into an
AUTOCAD schematic and consist of 25 sets of
micro-channels. Each one of the patterns is
illustrated in Fig. 1. These designed micro-
channels once fabricated would be linked to
several sets of electromechanically actuated
micro-pumps, which are designated to transport,
mix, or separate certain bio-fluids as well as
perform valve operations. The micro-pumps are
designed in an octagonal shape, which features
low residual stresses and high volume rate of
pumping efficiency. Stress analysis of the
micro-pump structures using a finite element
utility (ANSYS) is shown in Fig. 2. Exerted
pressure due to generated electromechanical
forces is designed to be 3 MPa, and simulation
results show that the maximum stress existing
around the edge of the pump membrane is
51.3 MPa, which is far below the yielding
strength of the membrane (230 MPa).
3. Wet-Etching Options for Micro-Channels
As for wet-etching solutions to fabricate
the micro-channels, several factors need to be
considered: 1. preparation readiness, 2. toxic
constitutions, 3. silicon etching rate, 4. etching
stopper mechanism, 5. etching selectivity, 6.
etching stopper thickness, and 7. etched-surface
profile roughness. These factors for commonly
adapted anisotropic wet-etching solutions are
listed in Table I.
Since the metal can be deposited using the
apparatus in our clean-room are limited for
certain materials, and aluminum is one of our
restricted options. Comparing the merits and
demerits of the listed wet-etching solutions in
Table I, TMAH is chosen in our research to do
the etching job for fabricating micro-channels,
and aluminum is selected to be the stopper
material for the etching process. In addition,
proper amounts of SiO
2
or silicon power are
added into the TMAH solution as to reduce its
attacking effect on aluminum, and ammonium
peroxodisulfate (AP) is also added to optimize
the roughness as well as flatness of the silicon
micro-channels etched surfaces for the.
Low resistance (<50 !) single-sided 4 silicon
wafers (100 direction) are used as substrates of
the micro-structures, and an RF-sputter is
employed to deposit thin layers of aluminum as
stopper mechanism for the etching processes.
The experimental deposition rate for the metal
sputtering is plotted in Fig. 3, and designated
thickness of the aluminum barrier layers is
optimized to be 100 nm. Thereafter, the
patterns on photomasks are transferred onto the
silicon wafers based upon lithography technique.
Then, on top of the aluminum layers a
developing solution AZ P4602 is exercised to
open some windows, as shown in Fig. 4, which
are designated to expose the silicon area to be
etched by TMAH. The flow chart to etch
through the opening windows is illustrated in
Fig. 5.
4. Micro-Channel Fabrication Processes
Literature surveys show that increasing
TMAH solution concentration would reduce its
etching rate on silicon matrix. TMAH etching
rate reaches its maximum as it has a
concentration of 0.4~0.5%wt, but the etched
surface would remain certain pits or bulges [11,
12]. The problem is solved by increasing the
TMAH solution concentration up to 20%wt, but
the etching rate is reduced down to 0.5~0.6 m
[11, 13]. On the other hand, adding AP to the
TMAH solution can reduce the bulge problems
as well as raise the etching rate for TMAH on
silicon matrix [14, 15]. Aiming to obtain
optimal micro-channel etched surfaces in this
research, a lab-prepared recipe of 5%wt
concentration TMAH solution, added with AP
and silicon power, is implemented to etch the
opened windows within the silicon matrix until
the deposited aluminum stopping layers are
MICRO-CHANNEL FABRICATIONS WITH TMAH ANISOTROPIC WET-ETCHING
3
encountered. Steps of micro-channel
fabrication processes using TMAH anisotropic
wet-etching solutions are listed in Table II.
Experiments were conducted as varying the
parameters related to the TMAH wet-etching
performances, and measurements as well as
evaluations for five experimental cases are
described in Table III.
5. Experimental Results and Discussions
In the experiments, all the TMAH solutions
used contain 5%wt concentration with different
ratios of silicon power and AP. Fig. 6 shows
the windows are etched in Case 1 condition, and
the depth is 30.81 m with a roughness of
145.6 nm after 30 minutes of etching. Fig. 7
shows the windows are etched with more silicon
power added as in Case 2 condition, and the
etched depth is 27.6 m with a roughness of
65 nm. Fig. 8 shows the windows are etched
with less silicon power added as in Case 3
condition, and it is observed the attacked
aluminum stopper layers are totally dissolved
after 5 min. 42 sec. of etching processes.
On the other hand, experiments with different
weightings of AP added into the TMAH
solutions are also carried out. When the added
AP weight ratio is 4g/L as in Case 1 condition,
the windows are etched into a 30.81 m depth
without any attack to the aluminum layer as
shown in Fig. 6. Fig. 9 shows the windows are
etched with more AP added up to 5g/L as in
Case 4 condition, and the etched depth is
29.4 m with a roughness of 131.7 nm. Fig. 10
shows the windows are etched with less AP
added down to 3g/L as in Case 5 condition, and
the etched depth is 30.72 m with a roughness
of 45.5 nm. The experimental observations
verify that weighting ratio of AP being lower
than 3g/L can cause TMAH solution attacking
on aluminum stopper layers. The roughness of
the etched micro-channel surfaces versus AP
weighting ratio as implementing a 5%wt TMAH
solution is tabulated in Fig. 11.
Hence the experiments results demonstrate that
the etching parameters in Case 5 can be adopted
to fabricate the micro-channels required in this
research. The etching processes would result
satisfactory surface roughness without any
attack on the aluminum layers. The
measurements of surface profile for the etched
micro-channel surfaces in Case 5 is shown in
Fig. 12, and it can promises leading to better
micro-fluid transportation behaviour during
subsequent micro-pumping operations.
6. Conclusions
The goal to fabricate micro-channel
profiles with great smoothness on silicon wafers
is accomplished based upon a modified TMAH
wet-etching recipe. Firstly in the processes
deposited aluminum layers are formed using a
PVD sputter, and proper adjustments of added
AP and silicon power constitutions can result in
fast etching rate without any attacking on the
aluminum layers. As well, micro-channel
surface roughness can be reduced to 45.5 nm for
subsequent micro-fluid operations.
References
[1] Tsaur, J. J., Du, C. H., and Lee, C. K., Investigation
of TMAH for front-side bulk micromachining
process from manufacturing aspect, Sensors and
Actuators A, Vol. 92, pp. 375-383, 2001.
[2] Lassen, E. H. K., Reay, R. J., Storment, C., Audy, J.,
Henry, P., Brokaw A.P., and Kovacs, G.T.A., ,
Micro-machined thermally isolated circuits,
Proceedings of the 1996 Solid-State Sensor and
Actuator Workshop, Hilton Head Island, S. C.
pp. 127-131, 1996.
[3] Lassen, E. H. K., Reay, R. J., and Kovacs, G. T. A.,
Diode-based thermal rms converter with on-chip
circuitry fabricated using CMOS technology,
Sensors and Actuators A, Vol. 52, pp. 33-40, 1996.
[4] Williams, K. R. and Muller, R. S., Etch rates for
micromachining processing, Journal of
Microelectromechanical Systems, Vol. 5, No. 4,
pp. 256-269, 1996.
[5] Williams, K. R., Gupta, K., and Wasilik, M., Etch
rates for micromachining processing-Part II, Journal
of Microelectromechanical Systems, Vol. 12, No. 6,
pp. 761-778, 2003.
[6] Pandy, A., Landsberger, L. M., Nikpour, B.,
Paranjape, M., and Kahrizi, M., Experimental
investigation of high Si/Al selectivity during
anisotropic etching in tetra-methyl ammonium
hydroxide, J. Vac. Sci. Technol. A, Vol. 16, pp. 868-
872, 1998.
[7] Lian, K., Stark, B., Gundlach, A .M., and Walton, A.
J., Aluminum passivation for TMAH based
Fu-Shin Lee, Chih-Hsiung Chen, Chiang-Chao Liao, Jyh-Ling Lin
4
anisotropic etching for MEMS application,
Electronics Letters 22
nd
, Vol. 35, No. 15, pp.1266-
1267, 1999.
[8] Yan, G., Chan, C. H., Hsing, I. M., Sharma, R. K.,
Sin, K. O., and Wang, Y. Y., An improved TMAH
Si-etching solution without attacking exposed
aluminum, Sensors and Actuators A, Vol. 89,
pp. 135-141, 2001.
[9] Fujitsuka, N., Hamaguchi, K., Funabashi, H.,
Kawasaki, E., and Fukada, T., Silicon anisotropic
etching without attacking aluminum with Si and
oxidizing agent dissolved in TMAH solution,
Sensors and actuators A, Vol. 114, pp. 510-515,
2004.
[10] Chen, P. H., Peng, H. Y., Hsieh, C. M., and Chyu, M.
K., The characteristic behavior of TMAH water
solution for anisotropic etching on both silicon
substrate and SiO
2
layer, Sensors and actuators A,
Vol. 93, pp. 132-137, 2001.
[11] Tabata, O., Asahi, R, Funabashi, H., Shimaoka, K.,
and Sugiyama, S., Anisotropic etching of silicon in
TMAH solution, Sensors and Actuators A, Vol.34,
pp.51-57, 1992.
[12] Thong, J. T. L., Choi, W. K., and Chong, C. W.,,
TMAH etching of silicon and the interaction of
etching parameter, Sensors and Actuators A,
Vol. 63, pp. 243-249, 1977.
[13] Merlos, A., Acero, M., BAusells, J., and Esteve, J.,
TMAH/IPA anisotropic etching characteristics,
Sensors and Actuators A, Vol. 37-38, pp. 737-743,
1993.
[14] Lassen, E. H. K., Reay, R. J., Storment, C., Audy, J.,
Henry, P., Brokaw A.P., and Kovacs, G.T.A.,
Micro-machined thermally isolated circuits,
Proceedings of the 1996 Solid-State Sensor and
Actuator Workshop, Hilton Head Island, S. C.
pp. 127-131, 1996.
[15] Lassen, E. H. K., Reay, R. J., and Kovacs, G. T. A.,
Diode-based thermal rms converter with on-chip
circuitry fabricated using CMOS technology,
Sensors and Actuators A, Vol. 52, pp. 33-40, 1996.

Figures and Tables

Fig. 1 Opening windows for etching



Fig. 2 Membrane stress distributions
using FEM analysis
times vs. deposition thickness
0
500
1000
1500
2000
0 500 1000 1500 2000
times(sec)
d
e
p
o
s
i
t
i
o
n
t
h
i
c
k
n
e
s
s
(

m
)

Fig. 3 Aluminum deposition rate


Fig. 4 Photo of etching windows
MICRO-CHANNEL FABRICATIONS WITH TMAH ANISOTROPIC WET-ETCHING
5

Fig. 5 Fabrication processes for etching
through opening windows


Fig. 6 Etched micro-channel profiles in Case 1:
5%wt TMAH with Si (14g/L) and AP (4g/L)


Fig. 7 Etched micro-channel profiles in Case 2:
5%wt TMAH with Si (16.5g/L) and AP (4g/L)


Fig. 8 Etched micro-channel profiles in Case 3:
5%wt TMAH with Si (11.5g/L) and AP (4g/L)

Fig. 9 Etched micro-channel profiles in Case 4:
5%wt TMAH with Si (14g/L) and AP (5g/L)
Fu-Shin Lee, Chih-Hsiung Chen, Chiang-Chao Liao, Jyh-Ling Lin
6

Fig. 10 Etched micro-channel profiles in Case 5:
5%wt TMAH with Si (14g/L) and AP (3g/L)


0
50
100
150
200
2 3 4 5 6
(NH4)2S2O8 Quantity(g/L)
S
i
l
i
c
o
n

S
u
r
f
a
c
e
R
o
u
g
h
n
e
s
s
(
n
m
)

Fig. 11 Roughness of micro-channel profiles for
various concentrations of AP in 5%wt TMAH


Fig. 12 Surface profile measurement for etched micro-channels in Case 5 after 30 minutes
Table I Comparison of anisotropic etching solutions
TMAH EDP KOH
Processing Easy Hard Easy
Toxicity N/A Yes No
silicon etching rate 1m/min 0.02~1m/min 1~2m/min
Etched surface
flatness
Varying Excellent Good
Compatibility with
IC fabrication
Yes Yes No
Boron etching stop >10
20
/cm
3
510
19
/cm
3
>>10
20
/cm
3

Other stopper
material selectively
Al Ta, Au, Cr, Ag, Cu N/A
Silicon etching
stopper
Si
3
N
4
, SiO
2
Si
3
N
4
, SiO
2
Si
3
N
4


MICRO-CHANNEL FABRICATIONS WITH TMAH ANISOTROPIC WET-ETCHING
7
Table II Fabrication processes for micro-channels using TMAH anisotropic wet-etching solutions
Step Fabrication Process
1 Pour silicon powder into a 2000mL beaker container.
2
Add 500mL de-ionized water into another larger beaker containing
300mL of 25% tetraethyl ammonium hydroxide solution and shake well.
3 Place the beaker on top of a stirrer and heat up to 80 in high blending condition.
4
If the mixture is clear, Add de-ionized water up to 1500mL scale
of the beaker container once the blended solution becomes transparent..
5
Add ammonium peroxodisulfate powder (AP) into the beaker
once the stirred solution becomes clear again.
6
Decelerate the stirring to appropriate speed when the mixture becomes clear again,
and place the silicon chips to be etched in the beaker to start etching.
7
Remove the chips after 30~40 minutes of etching.
Pput 8mL 25% TMAH more into the solution with 5g AP added subsequently.
Place the chips in the beaker again after 10 minutes waiting
for the solution to become clear again.
8 Repeat step 7 as many times as necessary to complete the etching processes.

Table III Compositions in TMAH solutions
Case
TMAH
concentration
Substances added
Silicon
etching rate
[100]
Aluminum
attacking
Roughness
Ra (nm)
1 5%wt Si (14g/L)+AP(4g/L) 1.027m/min No 145.6
2 5%wt Si (16.5g/L)+AP(4g/L) 0.920m/min No 65.0
3 5%wt Si (11.5g/L)+AP(4g/L) N/A Yes N/A
4 5%wt Si (14g/L)+AP(5g/L) 0.998m/min No 131.7
5 5%wt Si (14g/L)+AP(3g/L) 1.024m/min No 45.5