PROTOCOL TO BUILD 2D TRANSPARENT PDMS MICROMODELS FOR

USE IN DRYING EXPERIMENTS

Luis A. Segura, Guillermo M. Badillo, Fabiola V. Villagra and Daniela L. Garrido
Universidad del Bo-Bo, Food Engineering Department
Avda Andrs Bello S/N, Chilln, Chile, email: lsegura@ubiobio.cl
Keywords: flexography, transparent micromodels, porous materials, polydimethylsiloxane
ABSTRACT
Shrinkage during drying affects the porous shape and rehydration capability of any given
deformable porous structure. Moreover, only a few studies have been carried out to explain the
mechanisms that provoke shrinkage during drying. We postulate that shrinkage is mainly produced
through changes in capillary pressure during drying in a deformable porous structure. Subsequently,
if capillary pressure is mainly responsible for shrinkage in a pore structure, it is then necessary to
know the liquid phase distribution inside it as drying occurs. Transparent micromodels can be
defined as transparent networks of pores and constrictions that simulate some of the complexities of
natural porous media and are a useful tool to observe liquid distribution at pore scale. Micromodels
have traditionally been built in glass and resin and have been very useful tools to observe and
quantify liquid distribution and transport mechanisms involved in drying. Since they are built in
rigid materials, shrinkage can only be indirectly studied. , A new method based on the traditional
photolithographic technique has been developed to build deformable micromodels, which is an
elastomeric material called polydimethylsiloxane (PDMS). This study reports the protocol to build
2D deformable transparent PDMS micromodels for future applications in the drying process and
which is necessary to find evidence about transport properties directly related to shrinkage

INTRODUCTION
Several water transport mechanisms are involved during the drying of a pore structure.
These mechanisms are present at different stages of the process and depend on such factors as
solid/liquid/gas distribution, topology and morphology of the pore structure, and composition of the
wall pores (Laurindo and Prat, 1996, San Martin et al., 2011). The transparent micromodel is a
useful tool to observe liquid/gas distribution during drying at pore scale. According to Oyarzn and
Segura (2009), transparent micromodels can be defined as transparent networks of pores and
constrictions that simulate some of the complexities of natural porous media (see Buckley, 1991 for
a review). More generally, bead packs and single-pore models are micromodels. It is possible to
clarify the water transport mechanisms involved during drying of a pore structure through
micromodels because they show complex liquid/gas/solid interactions and the relationship of these
interactions with the pore space topology during the process. Although the use of micromodels has
produced advances in the comprehension of the phenomena associated with drying processes
(Laurindo and Prat, 1996, 1998; Tsimpanogiannis, et al., 1999; Oyarzn and Segura, 2009; Diaz et
al., 2011; Segura and Oyarzn, 2012; Vorhauer et al.., In Press), these micromodels have been built

from rigid materials such as glass or plexiglass (resin); therefore, they do not capture some
important features of a biological matrix such as flexibility and shrinkage. They also cannot provide
evidence of the transport properties directly related to shrinkage.
As previously mentioned, micromodels built of glass and resin have been very useful tools
to observe and quantify liquid distribution and transport mechanisms involved in drying; however,
since they are built of rigid materials, shrinkage can only be indirectly studied. , A new method
based on the photolithographic technique has been developed to build deformable micromodels,
which is an elastomeric material called polydimethylsiloxane (PDMS). With this kind of materials it
is possible to obtain micromodels with a pore radius value greater than 20 m over a short period of
time. Another important advantage of this kind of micromodel as compared with those built of glass
or resin is the possibility of building 3D micromodels (Anderson et al., 2000). The method consists
in modifying the classical photolithographic technique. Duffy et al. (1998) were the first to develop
the technique; some papers have been published since then (Mc. Donald et al., 2000; Jo et al., 2000;
Anderson et al., 2000, and Kim et al., 2009) that describe the method in detail. According to
McDonald et al. (2000) PDMS is an excellent material for the fabrication of microchannel
systems for use with biological samples in aqueous solutions for a number of reasons (i) features on
the micron scale can be reproduced with high fidelity in PDMS by replica molding; (ii) it is
optically transparent down to 280 nm so it can be used for a number of detection schemes (e.g.
UV/Vis absorbance and fluorescence); (iii) it cures at low temperature; (iv) it is nontoxic; (v) it can
be deformed reversibly; (vi) because it is elastomeric, it will conform to smooth, nonplanar
surfaces, and it releases from delicate features of a mold without damaging them or itself.
Polydimethylsiloxane micromodels have been applied in different fields such as chemistry
(Mogensen et al., 2003), biomedicine (Ki-Hum et al., 2006), physics (Studer et al., 2004),
nanotechnology (Ryu et al., 2004), micromolds (Parashar et al., 2002; Xia et al., 1996), microvalves
(Yoo et al., 2006; Abhinkar, 2007), microfluidic systems (Anderson et al, 2000; Mcdonald and
Whitesides, 2002), chemical sensors (Lowder et al., 2007; Wessling et al., 2001), biochip cells
(Baudoin et al., 2007; Marquette and Blue, 2004), gas transport systems (Stroock et al., 2002), and
chemical and microchemical analysis systems (Bruin, 2000). In each of these applications the
PDMS manufacturing process structures vary depending on the concentration of the base and curing
agent in the mixture (Ren et al., 2006), or the curing time modification proposed by the
manufacturer (Chronis et al., 2003; Jeong et al., 2004). Figure 1 shows the general outline of the
manufacturing process of the 2D PDMS microfluidic system with the technique proposed by Duffy
et al. (1998); Xia and Whitesides, (1998), and Qin et al. (1998).
Although PDMS systems have been applied to different disciplines, there is no evidence
about building network systems to study shrinkage during the drying process. This study aims to
develop a protocol for building 2D PDMS micromodels of deformable pore networks. This kind of
micromodel can be a useful tool to find evidence about the transport properties involved in the
shrinkage phenomenon of a given porous matrix.

Figure 1. (A) Rapid prototyping is the generation of a high-resolution transparency to be used as a

photomask. (B) Fabrication of the master involves spin-coating photoresist on a silicon
wafer and developing the photoresist through a photomask. (C) Replica molding involves
pouring a mixture of PDMS prepolymer and curing agent on the master, curing at 70 C for
1 h, and peeling the replica off the master. (Adapted from Jessamine et al., 2002).

MATERIALS AND METHODS

The following materials were used to construct the micromodels: photopolymer plate
(TOYOBO model KM43GS), Sylgar 184 Silicone Elastomer Base (Dow Corning), Sylgar 184
Silicone Elastomer Curing Agent (Dow Corning), Silica Gel, Acetate sheeting, commercial soda
plate glass (4 mm), and glass and plastic materials.
The following equipment was used: a flexo station consisting of an electric oven (model
Nex TO-16) adapted with a fan and an ultraviolet light projection camera. A temperature-controlled
oven (Shel-lab 1375 FX), Close Focus Microscope monocular 45x (Model 03098-00), Harrick
Plasma Cleaner (Harrick Plasma Company), Flowmeter (Model 032-15-N), vacuum pump (Trivac
D 2,5 E Oerlikon Leybold Vacuum, SA.), Analytical Balance (Precisa, model XB 320M), and a
Canon printer (Pixma, IP4910) were also used. Other handmade equipment such as a curing
chamber, a vacuum chamber, and a metal press were used.
The first step to manufacture the PDMS micromodels was to develop the pattern design
(matrix) with a pore size distribution of a selected material (e.g., apple, carrot, and potato). The next

step was to obtain the photopolymer plate mold. The summary of the step-by-step procedure is as
follows: The photopolymer was covered with the pattern (negative) of a porous system before
being exposed to ultraviolet light (UV). The photopolymer which did not react with the ultraviolet
light was then removed using water. Water selectively dissolves the areas that were not exposed to
ultraviolet light and leaves a porous structure printed in the photopolymer material. Next, the mold
was filled with Sylgard 184 and cured at room temperature to obtain a layer of PMDS porous
structure. Finally, a second plane layer (without pores) of Sylgard 184 was developed, joined, and
bound through air plasma to obtain the 2D PDMS micromodel. The manufacturing stages of the
deformable PDMS micromodel, along with modifications to the protocol developed by Duffy et al.
(1998); Xia and Whitesides, (1998) and Qin et al. (1998), are described in detail below.
1) Pattern design
To obtain micromodels that can capture the main geometrical and topological features of some
deformable materials (Karathanos et al., 1996; Daz et al., 2011), a Log-Normal pore size
distribution function with porous radii ranging between 60 and 360 m was selected (Figure 2)
A code in Visual Basic (version 6.0) was used (Oyarzn and Segura, 2009) to generate pore
radii values that obey a Log-Normal distribution function. The code was fed with statistical values
from the selected materials, i.e., mean value of 140 m, standard deviation of 40 m, maximum
radius of 330 m, and minimum radius of 60 m with 50 x 50 pores in accordance with the
procedure described by Oyarzn (2008).

Figure 2. Log-Normal pore size distribution function

Once the data from the pore size distribution function were generated, they were drawn with the
AutoCAD software (version 16.1, Autodesk Inc.). A graduated throat with values ranging from a
minimum radius of 60 m to a maximum radius of 360 m was added and connected to the network
pattern to measure the effect of shrinkage as a function of the capillary pressure and humidity
saturation of the network during a given drying process experiment. The photomask dimension was
8 x 6 cm, which is smaller than the photopolymer plate, but which allowed cutting the edges of the
PDMS layer to obtain regular borders and straight edges. Figure 3 shows a positive pattern of 50

50 pores with pores throat radii distributed according to a Log-Normal distribution function. Pore
throats (channels) are represented in white and the solid phase in black.

Figure 3. Network pattern generated in AutoCAD (50x50 pores, node-to node distance of 1 mm, and throat
radius of log-Normal between 60 and 360 m) with a graduated throat with values ranging between the
lowest and highest radius.

2) Developing photopolymer matrix

A 13 x 11 cm photopolymer plate (TOYOBO model KM43GS) was used to build matrix
support for the PDMS polymer. The photopolymer plate was aligned with the photomask shown in
Figure 3 and placed in the UV chamber for 4.5 minutes at a wavelength of 365 nm. Next, the
photopolymer plate was washed with a sponge and clean water at room temperature for 3 min and
the matrix was exposed 2 min to UV light to strengthen the structure.
Figure 4a shows the developed photopolymer matrix and Figure 4b shows a glass frame
(cuvette) where Sylgar 184 must then be poured.

(a)

(b)

Figure 4.(a) Matrix developed in the photopolymer ; b) Matrix developed with the glass frame (cuvette)

3) Conditioning of glass plates

This procedure is similar to the one described in a previous study (Daz et al., 2011). Glass
edges to the cuvette were buffed with sandpaper (400 grit sandpaper to water) to remove sharp
edges and eliminate scratches on the glass surface. Next, they were immersed in a solution
containing 2% of detergent.

The glass plates were cleared on both sides with a cotton swab and rinsed with abundant
running water to remove residual detergent.
The plates were then washed with distilled water to remove residual salts present in drinking
water. The plates were immediately transferred to an oven, where they were dried for 30 minutes at
150 C. To avoid contamination of the plate surfaces, they were attached with metal clips, which
were held to the oven rack.
4) Fabrication of PDMS Micromodel Device
The following procedure is described to develop the PDMS device (deformable micromodel):
25 ml of Sylgard 184 (base and curing agent) in a 10:1 ratio, respectively, was prepared in a Petri
dish. Subsequently, the mixture was shaken to ensure homogeneity between the base and the curing
agent and a vacuum was applied for 10 min to remove bubbles produced by agitating the mixture. It
was then poured into the cuvette (Figure 4b) and cured for 48 h at room temperature. Finally, the
mixture was cured at 145 C for 15 min in an oven at a controlled temperature.

(a)

(b)

Figure 5. (a) PDMS poured in the photopolymer matrix; (b) Porous PDMS layer after curing was finished (48
hours).

The procedure shown in Figure 5 was carried out to obtain the second plane layer (without
pores) of PDMS, but instead of using the photopolymer revealed matrix, a commercial soda glass
was used with the same dimensions of the photopolymer plate (13x11 cm).
5) Micromodel Bonding
The bonding process is described as follows: The two layers of PDMS (with pores and without
pores) were immersed in ethanol and then dried in a vacuum at room temperature in a desiccator for
1 h. Next, both PDMS layers were put in the Harrick Plasma Cleaner equipment (Figures 6a and 6b)
for 25 min at low pressure (200-300 mtorr) with a controlled airflow of 12 ml/min and at a
maximum power of 26.9 Watt. The plasma process changes the surface properties of elastomer by
adding free radicals on the surface of the PDMS layers; theses are nitrogen and oxygen in the case
of air plasma.
After the plasma process, the two PDMS layers were joined and placed in a metal press (Figure
6c) where a pressure of 3 Kgf was applied for 45 min at 75 C. Applying these conditions produces
an irreversible bonding of the two PDMS sheets to obtain a 2D transparent PDMS micromodel.

(a)

(b)

(d)
Figure 6. (a) Plasma Cleaner Chamber; (b) PDMS layer inside the plasma chamber; (c) Irreversible
sealing of PDMS sandwich at a pressure of 3 Kg f in an oven at 75 C for 45 min.

RESULTS AND DISCUSSION

From a subroutine in Visual Basic (version 6.0) and available statistical data of a given
porous material (maximum and minimum throat radius, mean, and standard deviation), pore size
distributions and network images were generated using the AutoCAD software. Figures 7a, b, and c
show a 2D PDMS micromodel built in the present study. The micromodel was developed with a
Log-Normal pore size distribution function with porous values ranging between 60 and 360 m.
Figures 7d, e, f, and g show images of micromodels built from different materials such as glass and
resin in order to compare the results obtained in the present study with those available in the
specialized literature. Figure 7d shows a glass micromodel obtained by Zamorano (2007), Figures
7e, and f show a resin micromodel obtained by Diaz et al., (2011), and Figure 7g shows a resin
micromodel developed by Bonnet and Lenormand, 1977.
Comparing the micromodel built in the present study with glass micromodels, the PDMS
micromodel displays channels (pore throats) with better pore straight cuts and better resolution than
the others (Oyarzn and Segura 2009). By comparing images from Figure 7 it is possible to see that
the glass micromodel (Figure 7d) has irregular channels produced by acid attack; this is compared
with the high resolution achieved in the channels produced with PDMS (Figure 7c). Figure 7f
shows a resin micromodel developed by Diaz et al., (2011) where a good resolution was also
obtained. When comparing the three materials, it can be seen that the resolution was improved for
PDMS micromodels because the micromodel pattern obtained in the present study has a square

configuration, while those obtained by Bonnet and Lenormand (1977) had an almost completely
circular shape.
Another important achievement of the present study is a constant throat depth compared
with other micromodel manufacturing techniques. The throat depth of the micromodels obtained in
the present study was 0.233 mm.

(a)

(b)

(c)

(d)

(e)

(f)

(g)
Figure 7. a) 2D PDMS micromodel; b) deformability of the micromodel developed with the protocol in this
study; c) zoom of the pore structure d) Glass micromodel (Zamorano, 2007); e) and f) Resin micromodel
developed by Diaz et al,,(2011); g) micromodel built by Bonnet and Lenormand (1977).

The most important feature of the PDMS micromodel built in the present study as compared
with the others shown in Figure 7 is its capacity to be deformed when subjected to a stress
condition, such as shrinkage, during a drying process. The micromodel that was built contains a
graduated channel (Figure 3) that can measure variations with capillary pressure as drying occurs.
Finally, there is no evidence in the specialized literature related to the use of this kind of
PDMS micromodels to study the drying process, but there is evidence of the use of these materials
in the development of microfluidic systems (see Jessamine et al., 2002 for further review). The
general protocol for the manufacture of micromodels used in the present study is detailed as
follows:

Figure 8. Diagram of the technique developed for manufacturing the deformable micromodel

CONCLUSIONS
A protocol to obtain 2D PDMS micromodels based on the modified protocol developed by Diaz et
al., (2011), Duffy et al., (1998), Xia and Whitesides, (1998) and Qin et al., (1998) was
implemented.
The micromodels have the following characteristics: straight cuts of the solid matrix, throat depth of
232 m, and node to node distance of 1 mm. Additionally, deformable 2D PDMS micromodel
captures the main feature of the biological material when subjected to drying, which is contraction
(shrinkage effect) . It is also possible to extend this use to other natural materials. The micromodel
that was built contains a graduated channel that can measure variations with capillary pressure as
drying occurs. Therefore, future research will be focused on studying the effects of capillary
pressure on shrinkage during drying of a pore structure using this kind of micromodel.

ACKNOWLEDGEMENTS
This study was funded by FONDECYT Grant #1120347.

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