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Theoretical and experimental studies on the


parylene diaphragms for microdevices

Article in Microsystem Technologies · August 2005


DOI: 10.1007/s00542-003-0342-7

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Microsystem Technologies 11 (2005) 11–15  Springer-Verlag 2005
DOI 10.1007/s00542-003-0342-7

Theoretical and experimental studies on the parylene diaphragms


for microdevices
W. Sim, B. Kim, B. Choi, J.-O. Park

11
Abstract In this paper, parylene diaphragms with planar Moreover, since parylene is bio-compatible, many
and corrugated shapes are fabricated and tested. Although, researchers have used it for a diaphragm material [5]. In
recently in MEMS, parylene has been used for a diaphragm spite of frequent uses for applications in micromachined
material due to its excellent property, no theoretical and devices, the analytical and experimental study of parylene
analytical studies of the parylene diaphragm have been diaphragm has never been performed. It is important to
performed. Therefore, the characterization of the parylene figure out the accurate behavior of the parylene diaphragm
diaphragms is studied through both experiments and in order to design the microfluidic components such as
simulations. Thermal and load-deflection analyses for micopumps and microvalves.
diaphragms are carried out to find the effect of residual For most applications, membrane is required to achieve
stress on the behavoir of the diaphragm. The measured a large displacement to transfer some pressure into
deflections are compared with both analytical calculations working fluid. However, large initial stress can lead to
and FEM simulations that considers the influence of the undesirable effects that make the diaphragm hard to
thermal stress. Those results show excellent agreement. In deflect. The many reason for residual stress are studied
order to find an optimum shape of the corrugated dia- and reported. The major one is the difference in thermal
phragm, the influence of the corrugation number and the expansion coefficients between two layers [6, 7]. One way
corrugation depth on the mechanical sensitivity of the to reduce the influence of the internal stress is to use
corrugated diaphragm is studied parametrically. corrugations in a diaphragm [1, 8]. For corrugated dia-
phragm structures, the effects of the residual stress cannot
Keywords Parylene, Diaphragm, Thermal stress, FEM,
be analyzed easily because of the complex structure and
Optimum shape
non-uniform stress distribution profile. Therefore, FEM
analysis is needed in modeling and simulating corrugated
Introduction
diaphragm. In this paper, the planar and corrugated par-
Silicon, metal and silicone rubber, etc. are generally used
ylene diaphragms are fabricated and tested. Using load-
as the membrane material for microsystem applications
deflection method, the residual stresses of diaphragms are
[1–3]. The diaphragm of silicon or metal is relatively stiff
obtained and experimental results are compared with
and does not make a large displacement. However, par-
analytica l and FEM results. The commercial finite-element
ylene is waterproof and much more flexible than silicon
code, CoventorWareTM , is employed to obtain the thermal
and it is possible to deposit other layers on it [4].
stress and the deflection of diaphragms corresponding to
the variation of applied pressures.
Received: 27 June 2003 / Accepted: 31 August 2003
Design and fabrication
W. Sim, J.-O. Park In this paper, two kinds of diaphragms are fabricated by
Intelligent Microsystem Center, using anisotropic etching technique. The one is the flat
P.O. Box 131, Cheongyang, Seoul, 130–365, South Korea diaphragm and the other is the corrugated one. Corruga-
tions of the parylene diaphragm are suggested to increase
B. Kim the deflection of the diaphragm by reducing the initial
Microsystem Research center, stress. The size of the square flat diaphragm is
Korea Institute of Science and Technology, P.O. Box 131, 2.8  2.8 mm2 or 4.3  4.3 mm2 . Also, the corrugated dia-
Cheongyang, Seoul, 130–365, South Korea
phragm of 4.3  4.3 mm2 with 5 corrugations is fabricated
B. Choi (&) and tested to compare with flat one. The thickness (t) of
Department of Mechanical Engineering, the corrugated diaphragm is 3 lm which is the same as
Sogang University, #1 Shinsu-dong, Mapo-gu, that of flat one. The schematic cross-sectional view of the
Seoul 121–742, South Korea corrugated diaphragm is shown in Fig. 1 and its charac-
e-mail: bkchoi@ccs.sogang.ac.kr teristic parameters are listed in Table 1. The width (w) and
depth (H) of the corrugation are 80 and 20 lm, respec-
The authors would like to thanks to Dr. Sang Sik Yang and
coworkers in the Microsystems Lab., School of Electronics tively.
Engineering, Ajou University for the help with device processing. The fabrication steps of the corrugated diaphragm are
This research was sponsored by Institute for Applied Science and shown in Fig. 2. The process starts with an n- type(100)
Technology of Sogang University. silicon wafer. The circular corrugations are first etched by
Fig. 1. The schematic cross-sectional view of the corrugated
parylene diaphragm

Table 1. The characterisrtic parameters of the corrugatd


dipaphragm
12
Parameter Symbol Value

Radius a 2.15 mm
Diaphragm thickness t 3 lm
Corrugation depth H 20 lm Fig. 3. The enlarged view of the corrugated diphragm. a The
Corrugation arc length S 209 lm buckled portion before removal of oxide. b The diaphragm after
Corrugation pitch P 160 lm etching the residual stress
Corrugation width w 80 lm

Fig. 2. The fabrication process. a Oxidation (6000 Å). b Corru-


gation etch (20 lm). c Parylene deposition (3 lm). d Backside
etch in EDP. e Oxide removal
Fig. 4. SEM photographs for the corrugated parylene diaphragm.
a The corrugation of the diaphragm. b The parylene layer 3 m
20 lm into the frontal surface of the silicon using ethylene thick
diamine pyrocatechol (EDP) solution. For flat diaphragm,
this corrugation etching is omitted. After removing the shown in Fig. 3. Figure 3a illustrates the buckled portion
silicon dioxide, another silicon dioxide layer of 0.6 lm of diaphragm due to a compressive stress of silicon
thickness is thermally grown again. Parylene-C of 3 lm dioxide under the parylene layer. The stretched parylene
thickness is deposited by using parylene deposition system diaphragm with tensile stress after removing the residual
(Labcoater, PDS 2010, SCS Inc.). During this process, oxide is shown in Fig. 3b. The SEM photographs of the
temperature and pressure in the deposition chamber are cross sectional view are shown in Fig. 4a and 4b, respec-
25  C and 0.1 torr, respectively. Under these conditions, tively.
the parylene polymer can be formed as continuous films The stress induced by the process of parylene deposi-
due to the vapor phase deposition. Afterward, the backside tion can be neglected because the temperature in reaction
of the wafer is patterned and silicon is etched away in EDP chamber does not rise more than a few degrees above the
solution using the silicon dioxide as an etch-stop layer. ambient. Therefore, it is considered that temperature
Finally, the residual oxide under the parylene layer is re- change, DT = 75  C, during silicon wet etching process is
moved using buffered oxide etching (BOE) solution. The the major reason for the residual stress of the parylene
enlarged view of the fabricated parylene diaphragm is layer.
Theoretical analyses
The difference in thermal expansion coefficients between
silicon substrate and parylene layer causes the thermal
stress when temperature changes occur. The thermal
expansion coefficients of silicon and parylene are
2.6  106 / C and 3.5  105 / C, respectively. During the
silicon etching process in EDP etchant, the temperature is
increased up to about 100  C. Therefore, the temperature
change, DT = 75  C, causes the residual stress which is a
very important factor for diaphragm performance. The Fig. 6. A deflected square diaphragm due to applied pressure
physical and mechanical properties of parylene-C are 13
presented in Table 2. Poisson’ s ratio of parylene is
assumed to be 0.4. The theoretical thermal strains due to
temperature change are as follows:
rx  tpa rz
epa ¼ ðasi  apa ÞDT; esi ¼ asi DT and epa ¼
Epa
ð1Þ
where e is the thermal strain, a the thermal expansion
coefficient, r the thermal stress, E Young’s modulus, and m
the Poisson’ s ratio. The parylene layer on the silicon
Fig. 7. Experimental setup for pressure-deflection mesurement
substrate is modeled as a biaxial state as shown in Fig. 5.
With an assumption of rx ¼ rz and strain compatibility
(ex ¼ ez ), we have tr tE 3
pðhÞ ¼ C1
h þ C2 ðvÞ 4 h ð4Þ
rx  vPa rz a2 a
asi DT  apa DT ¼ ð2Þ
Epa where C1 and C2 (m) are numerical constants, p is the
applied pressure, h the center deflection, a one half of the
Thus,
edge length, t the thickness. The value of the C1 is 3.45 and
Epa C2 can be written in the form C2 (m) = 1.994(1-0.271m)/
rx ¼ rz ¼ ðasi  apa ÞDT ð3Þ (1m) [9]. Equation (4) is derived with the assumption of
1  mpa
large deflection of thin films(h>>t). The measured
The load-deflection method is well known technique to deflections of flat diaphragm with respect to applied
determine the residual stress of the membrane structure. A pressures are compared with analytical and FEM results.
square flat diaphragm under applied pressure is shown in Also, on the basis of known data such as measured
Fig. 6. Theoretically, the relationship between the pres- deflections and applied pressures, the residual stress (r) is
sure, p, and the center deflection of the flat square dia- compared with the thermal stress calculated by both
phragm, h, is as follows: Eq. (3) and simulation.

Table 2. The properties of parylene-C Experiment and simulation


The experimental setup for load-deflection relation of
Property Value diaphragm is shown in Fig. 7. The parylene diaphragm
mounted on the pressure chamber is tested under various
Density 1.289 g/cm3 pressures and then the corresponding deflections are
Young’ s modulus 4.5 Gpa measured by using a laser displacement meter(KEYENCE-
Poisson’ s ratio 0.4 LC 2420). The applied pressure is monitored by a digital
Thermal expansion coefficient 3.5 · 10)5/C
display(INSTECH SM-50) which is connected to a pressure
Tensile strength 69 MPa
Melting point 290 C sensor. Also, the pressure level is controlled by a syringe
pump(KDS 100 kd Scientific co.).
The commercial finite-element code, CoventorWareTM ,
is used for the simulations. The 3D models are created for
both flat and corrugated diaphragms. In order to reduce
the computation time, a quarter symmetric modeling
technique is employed. For solving the governing differ-
ential equation, FE model for the flat diaphragm is meshed
with brick elements and the tetrahedral elements(free
meshing) are taken for the corrugated diaphragm because
of its complex geometry. In the procedure of FEM analysis,
first, thermal analysis is performed on the constructed 3D
model with known material properties and symmetric
Fig. 5. A biaxial model for parylene on the silicon substrate boundary conditions. Afterward, the given pressures are
Fig. 10. Simulated stress distribution, at DT=75  C. Quarter
14 symmetry model. All units are in MPa. a Contour plot for the flat.
b Contour plot for the corrugated
Fig. 8. Comparison of measured results among flat (2.8 mm2 ),
flat (4.3 mm2 ) and corrugated (4.3 mm2 ) diaphragms

Fig. 11. Comparison among theoretical, measured and simulated


deflections of flat diaphragm (4.3 mm2 ) with residual stress,
Fig. 9. The residual stress of the flat diaphragm according to 18.2 MPa, corresponding to the various pressures
differences in Temperature
With a consideration of 18.2 MPa initial stress, the
comparisons among the experimental, analytical and
applied to the pre-stressed diaphragm. Thus, the super- simulated load-deflection results of flat diaphragms with
position technique is used to analyze the effect of internal the sizes of 4.3  4.3 mm2 are shown in Fig. 11. Also, the
stress on the behavior of the parylene diaphragm. effect of residual stress is examined by comparing exper-
imental results with the theoretical results without con-
Results and discussion sidering the effect of residual stress. The results show that
Figure 8 shows the displacements of the flat and corru- the measured deflection is about a half of the deflection of
gated diaphragms under the various pressures. The the stress-free diaphragm at 3 kPa. The theoretical and
deflections of the flat and corrugated diaphragms with the simulation results that consider the internal stress show
size of 4.3  4.3 mm2 are 40 and 200 lm under 1.5 kPa, excellent agreement with the experimental values. There-
respectively. Compared with other materials, parylene fore, our prediction that the thermal stress is mainly
diaphragm has achieved relatively large displacement at caused by the thermal process is proved to be correct.
the same level of pressure due to its low Young’ s modulus. Some deviations between FEM analyses and experiments
The thermal stress on the parylene layer caused by the are considered to be measurement errors.
difference in thermal expansion coefficients is obtained by Based on the experimental and FEM results of the flat
analytical and finite-element calculations and the results diaphragm, we could know FEM analysis is a reliable
are compared in Fig. 9. After temperature approach for this problem. Therefore, deflection of a
change(DT = 75  C) occurs in the silicon wet etching corrugated diaphragm under various pressures is simu-
process, the residual stress of the flat diaphragm is ana- lated and compared to experimental results as shown in
lytically 18.2 MPa. Figure 10 shows the stress distribution Fig. 12. Our simulation results are well matched with
over one quarter of the flat and corrugated diaphragms at measurements. In this case, the deflection of the corru-
DT = 75  C. The internal stress on the flat diaphragm is gated diaphragm is much larger than that of the flat one
uniformly distributed. For the corrugated diaphragm, under the same pressures because the corrugations reduce
however, the value of stress on the center of the diaphragm the residual stress significantly. However, as we know in
is almost zero and it is increased as it goes to the edge. Fig. 12, the effects of internal stress regarding to deflection
According to the thermal FE analysis, it is known that still cannot be ignored. Thus, to improve the load-deflec-
corrugation structure prevents the stress from taking place tion performance of the corrugated diaphragm, the para-
and this effect is made, in particular, at the flat zone lo- metric study on the influence of the corrugation number
cated in the middle of the diaphragm. Therefore, great and corrugation depth on the mechanical sensitivity is
increase in displacement is achieved. performed. The mechanical sensitivity is defined as the
have been presented. According to the results, it has been
proved that the residual stress on parylene layer is mainly
induced by not parylene deposition but silicon wet etching
process since the thermal expansion coefficient of the
parylene is more than 10 times that of silicon. This internal
stress significantly affects the load-deflection relationship
of both flat and corrugated diaphragms. Compared with
flat diaphragm, the corrugated structure reduces the
residual stress dramatically and increases the deflection
more than 5 times. Namely, a pre-stressed flat diaphragm
has more rigidity than a corrugated one. Therefore, in
15
order to reduce the influence of the residual stress, the
Fig. 12. Comparison of the simulated and measured deflection of parametric FE study has been investigated and the
the flat and corrugated diaphragm (4.3 mm2 ) according to various improved mechanical sensitivity has been obtained.
applied pressures
The measurements are consistent with simulation
results, which show that FE methods could be applicable to
predict the behavior of both planar and corrugated
parylene diaphragm. Thus, this work helps to understand
the accurate behavior of the parylene diaphragm in terms
of load-deflection relationship and it could be used as a
guideline in designing the optimum shape of the
diaphragm for applications to micromachined devices.

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Conclusions
The first experimental and analytical study on the parylene
diaphragms has been performed and their characteristics

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