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Journal of Advanced Mechanical Design,Systems, andManufacturing
Vol. 2, No. 4, 2008
560
Micromachining of Soft Polymer Material
applying Cryogenic Cooling*
Yasuhiro KAKINUMA**, Nobuhito YASUDA** and Tojiro AOYAMA** **Dept. of System Design Engineering, Faculty of Science and Technology, Keio University,
3-14-1 Hiyoshi, Kouhoku-ku, Yokohama, 223-8522, Japan
E-mail: [email protected]
Abstract
Polydimethylsiloxane (PDMS) is one of the important materials for microfluidic
chips. The pattern of micro channels on the PDMS plate is usually fabricated
through the photolithography and micro molding process. However, the
photolithographic method requires multi chemical and mechanical processes and
resultant long process time. The micro milling process is a feasible method forrapid fabrication of various patterns of micro channels .However, micromachining
has not yet been applied to soft polymer materials. It is difficult to machine elastic
materials such as PDMS because of their low toughness. In order to machine a
micro grooves on soft polymer materials, the cutting process applying cryogenic
cooling is proposed because the elastic properties of soft polymer materials
remarkably change from rubbery state to glassy state below the glass transition
temperature. In this study, the freezing milling method using liquid nitrogen is
applied to the micro grooving of PDMS. The result of a cutting test shows that
micro grooves can be shaped easily and machined accurately in PDMS by the
proposed method.
Key words: Micromachining, PDMS, Cryogenic Cooling, µ-TAS, Microfluidic
Chip
1. Introduction
Recently, the study of µ-TAS (micro total analysis system) has developed rapidly and its
achievements have become the center of attention in the fields of micro fluidics and
biochemistry. The µ-TAS system, formed on one microfluidic chip [1, 2], consists of a
capillary that is a flow channel of liquid containing a sample and reagent, a reaction space
and a detection space. This system is expected to save micro samples, speed up the analysis,
automate the measurement, render the device portable, and reduce analysis costs.
The microfluidic chip used for µ-TAS is manufactured mainly from glass plate and the soft
polymer resin PDMS (polydimethylsiloxane) [3]. PDMS has been applied to crucial
components of micro devices in state-of-the-art research in bioengineering or micro
fluidics. The pattern of micro channels is usually fabricated through the micro molding
process, in which the micro molds are made by photolithographic methods. The
photolithographic method consists of the masking process, photoresist exposure and etching
processes, shown in Fig. 1. Although highly accurate processing is possible using
photolithography, the processing time lasts several days because of the multi process and its
need for a great amount of energy and hazardous chemicals is detrimental to the
environment. Other approaches, therefore, are required to manufacture a microfluidic chip
with high productivity and easier processing. The micro machining process, which is a
direct patterning method and is environmental friendly, is one of the potential approaches
for manufacturing microfluidic chips. Micromachining can provide a short turn around time*Received 21 Mar., 2008 (No. 08-0205)
[DOI: 10.1299/jamdsm.2.560]
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Vol. 2, No. 4, 2008
Si platePatterning photoresist
(Si Mold)
Thermosetting PDMS
Micro groove formed
Si
Mask
PDMSPhotoresist coating
Development
Figure 1: Multi process of photolithography
for manufacturing and produce three-dimensional channel shapes. The purpose of this study
has been to develop the micro milling technology of soft polymer materials such as PDMS
in order to manufacture microfluidic chips. It is difficult to machine the PDMS at room
temperature because of the low hardness of PDMS. On the contrary, below the glass
transition temperature its hardness increases suddenly and, in this state, it is expected that
PDMS can be precisely machined. Therefore, in this study, to realize PDMS machining,cryogenic cooling with liquid nitrogen was applied and the performance of the cryogenic
milling process for PDMS was experimentally evaluated.
2. Property of polymer materials
Polymer materials have a glass transition temperature, which depends on the main chain
structure of the polymer. At the glass transition temperature, the polymer changes from a
rubbery state to glassy state. Table 1 shows the glass transition temperatures for several
polymer materials. The glass transition temperature of PDMS is lower than that of any other
polymer material. Figure 2 shows the molecular architecture of PDMS and the PMMA
(polymethylmethacrylate). In PDMS, the main chain is Si-O bonding. The Si-O bonding
makes molecular motion easy because the atomic radius of silicon is larger than that of
carbon. Therefore, the glass transition temperature of PDMS becomes very low.This study proposes a new machining technology for elastic polymer material.
Specifically, this study proposes the micromachining of PDMS after it is cooled below the
glass transition temperature with liquid nitrogen. The temperature of liquid nitrogen is
lower than –196˚C. Since PDMS changes its state from rubbery to glassy when cryogenic
cooling is applied, it is expected that its machinability is improved.
Table 1: Glass-transition temperature of polymers
Glass-transitiontemperature centigrade
Polydimethylsiloxane -123
Polyethylene -30Polypropylene -10
Polymethylmethacrylate 105
Polycarbonate 150
Nylon 66 60
Glass-transitiontemperature centigrade
Polydimethylsiloxane -123
Polyethylene -30Polypropylene -10
Polymethylmethacrylate 105
Polycarbonate 150
Nylon 66 60
Si O
CH3
CH3
CH2 C
C=O
CH3
O
CH3
(a) PMMA (b) PDMS
Si O
CH3
CH3
CH2 C
C=O
CH3
O
CH3
Si O
CH3
CH3
Si O
CH3
CH3
CH2 C
C=O
CH3
O
CH3
CH2 C
C=O
CH3
O
CH3
(a) PMMA (b) PDMS
Figure 2: Molecular structure of PMMA and PDMS
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Vol. 2, No. 4, 2008
0
10
20
30
40
50
60
70
80
90
100
温 液 窒素 アクリル
H a r d n e s s ( J I S K 6 2 5 3 T y p e A )
PDMS atroom temperature
PDMS atultralow temperature
PMMA atroom temperature
0
10
20
30
40
50
60
70
80
90
100
温 液 窒素 アクリル
H a r d n e s s ( J I S K 6 2 5 3 T y p e A )
PDMS atroom temperature
PDMS atultralow temperature
PMMA atroom temperature
Figure 3: Hardness of the PDMS at room temperature and at ultralow temperature
Table
Dynamometer
Bakelite flame
Water circulationsystem
End millPDMS
Liquid nitrogenchamber
Liquid nitrogen
6 0 m m
110mm
Workpiece holder
: Temperature-measured point
Figure 4: Structure of cryogenic jig
PDMS
Water
Cryogenic cooling fixture
Micro square end mill
PDMS
Water
Cryogenic cooling fixture
Micro square end mill
Figure 5: Appearance of cryogenic machining system
3. Applying cryogenic cooling to the cutting process
3.1 Design of a special jig for cryogenic cooling
The change of hardness is measured by a durometer when the PDMS is cooling down with
liquid nitrogen. Figure 3 shows the hardness of PDMS at room temperature and at ultralow
temperature (below the glass transition temperature) and PMMA at room temperature. It is
clear that the hardness of PDMS at ultralow temperature is much higher than that at roomtemperature and the property of PDMS under cryogenic cooling changes into an acrylic. In
other words, PDMS changes from elastic to hard with cryogenic cooling.
In order to apply cryogenic cooling to the cutting process, a special jig with a liquid
nitrogen chamber was designed. The structure of the jig is shown in Fig. 4. The reservoir of
liquid nitrogen and the workpiece holder stage placed at the center of the reservoir are made
of aluminum because of its high heat conductivity. The PDMS plate is set on the stage and
fixed by an aluminum clamper. On the contrary, the outer flame made of bakelite has the
important role of insulating the heat transfer and suppressing the change of liquid nitrogen
to gas. The cutting force is measured by a dynamometer positioned under the special jig. To
keep the temperature at the bottom face of the jig constant and to prevent generation of the
heat drift of the dynamometer, a water circulation system is incorporated between the jig
and dynamometer. A photo of the special jig is shown in Fig. 5.
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Journal of Advanced Mechanical Design,Systems, andManufacturing
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Vol. 2, No. 4, 2008
-200
-150
-100
-50
0
50
0 500 1000 1500 2000 2500 3000
Time s
T e m p e r a t u r e
Adding the liquid nitrogen No liquid nitrogen
Under the water circulation system
Aluminum
Machining space
PDMS surface
-200
-150
-100
-50
0
50
0 500 1000 1500 2000 2500 3000
Time s
T e m p e r a t u r e
Adding the liquid nitrogen No liquid nitrogen
Under the water circulation system
Aluminum
Machining space
PDMS surface
Figure 6: Temperature property of the cryogenic jig
3.2 The heat characteristic of the special jig
To evaluate the heat characteristic of the jig before cryogenic cutting test, the temperatures
at four points of the jig were measured using a T-type thermocouple. The four measurement
points are on the aluminum stage, in the machining space, under the water circulation
system and on the surface of PDMS. In this evaluation, the end mill is away from the jig.
The results of the measurements are shown in Fig. 6. Whenever the liquid nitrogen
evaporates spontaneously and its amount diminishes, new liquid nitrogen is infused into thereservoir by manual operation. As the result of this operation, it takes approximately 1000
seconds for the temperature to reach steady state. After the steady state, the temperature of
PDMS is kept below the glass transition temperature, although it changes repeatedly
between -170˚C and -196˚C. It is estimated that this temperature change is caused by the
quantity of liquid nitrogen in the reservoir. The temperature of PDMS dipped in liquid
nitrogen is nearly -196˚C. On the other hand, when the amount of liquid nitrogen decreases
and PDMS also comes out from the liquid nitrogen, its temperature rises to approximately
-170˚C.
These results indicate that the developed jig is capable of cooling down PDMS below the
glass transition temperature and can be used as the cooling system for cryogenic machining
of PDMS.
4. Effect of applying cryogenic cooling in the cutting process
4.1 Experimental setup and procedure
The prepared sample of PDMS is produced by curing the mixed two components at room
temperature under a vacuum of 10kPa. The size of the PDMS sample is 20mm × 30mm ×
5mm (Width × Length × Thickness).
Using the developed jig, a cryogenic micro milling test of PDMS was carried out. The
cutting condition is summarized in Table 2 [4,5]. A three-axis vertical machining center
(NVD1500, Mori Seiki) was used. The non-coated micro square end mill with helical angleof 30˚ (RSE230, NS Tool), shown in Fig. 7, was used for the grooving operation. This end
mill is made of tungsten carbide. The diameter of the milling tool with two cutting edges is
0.5 mm. To investigate the difference between the cutting performance at room temperature
and at ultralow temperature, the cutting force in each condition was measured. Also, the
machined surface and shape were evaluated at room temperature using scanning electron
microscope (SEM) (VE7800, KEYENCE) and the 3D optical profiler (New View 6200,
Zygo).The SEM used in this study can observe the insulating material without Au or Pt
coating, applying low acceleration voltage. The optical profiler, based on the scanning
white-light technology, can measure the surface roughness with resolution of 0.1nm in
vertical direction. The measurement area of this profiler is 500µm × 700µm.
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Table 2: Cutting condition of PDMS at room temperature and at ultralow temperature
Rotational speed
Feed rate
Feed per tooth
Tool
Diameter of tool
WorkpieceMachine tool
5000min-1
10.0mm/min
1.0µ
m
Micro square end mill
0.5mm
PDMS3-axis vertical type
(b) Bottom of edge(a) Side view
100µm 66.6µm
(b) Bottom of edge(a) Side view
100µm100µm 66.6µm66.6µm
Figure 7: Micro square end mill ( 0.5)
-0.8
-0.6
-0.4
-0.2
0.0
0.2
0.4
0.6
0.8
1.0
0 0.01 0.02 0.03 0.04 0.05
Time s
C u t t i n g f o r c e i n f e e d d i r e c t i o n N At room temperature
At ultralow temperature1 revolution
-0.8
-0.6
-0.4
-0.2
0.0
0.2
0.4
0.6
0.8
1.0
0 0.01 0.02 0.03 0.04 0.05
Time s
C u t t i n g f o r c e i n f e e d d i r e c t i o n N At room temperature
At ultralow temperature1 revolution
Figure 8: Cutting force at room temperature and ultralow temperature
4.2 Result of cutting test
4.2.1 Cutting force
Figure 8 shows the behavior of the cutting forces in the feed direction both at room
temperature and at ultralow temperature. At room temperature, the cutting force is not
periodic and the absolute value is so low that the milling process could not be performed.
On the contrary, the cutting force in the cryogenic condition is larger than that at room
temperature and changes periodically in synchronization with the rotation of the milling
tool. This result confirms that the machining process can work on PDMS under the
cryogenic condition.
4.2.2 Evaluation of the machined surface
Figure 9 shows the shape of the machined groove observed by SEM as long as the PDMS
warm to room temperature after cryogenic cutting test. Although the PDMS cannot be cut at
room temperature, it can be machined in the cryogenic condition and the micro groove is
precisely formed. In order to investigate the machining accuracy, the shape of the groove
was evaluated using image measurement software. The actual width of the machined groove
is approximately 560 µm and the depth is approximately 200 µm. The desired shape is
500 µm wide and 200 µm deep. Both tool runout and the difference of shrinkage between
end mill and PDMS under ultra low temperature causes the machining error. The tool
runout was nearly 20µm in this test, measured statically by dial gauge with resolution of
1µm. Therefore, it is necessary to suppress the tool runout and consider the difference of
shrinkage between tool and workpiece for accurate machining.
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Top view
100µm100µm100µm
100µm100µm100µm 66.6µm66.6µm66.6µm
100µm100µm100µm
Top view
Side view
(a) At room temperature
Side view
(b) At ultralow temperature
Figure 9: Shape of machined groove (PDMS)
Table 3: Cutting condition for evaluation of machining characteristics
at room temperature and at ultralow temperature
Rotational speed
Feed rate
Feed per tooth
Depth of cut
Tool
Diameter of tool
Workpiece
Machine tool
5000min-1
1.0,10.0,50.0,100.0mm/min
0.1, 1.0, 5.0, 10.0µm
100µm
1000,5000,10000,20000min-1
10.0mm/min
5.0, 1.0, 0.5, 0.25µm
100µm
Micro square end mill
0.5mm
PDMS
3-axis vertical machining center
5000min-1
10.0mm/min
1.0µm
10,50,100,200µm
Feed rate change Rotational speed change depth change
-2.0
-1.5
-1.0
-0.5
0.0
0.5
1.0
1.5
2.0
0 0.01 0.02 0.03 0.04
Time s
C u t t i n g f o r c e i n f e e d d i r e c t i o n N
100.0mm/min
1.0 50.010.0
-2.0
-1.5
-1.0
-0.5
0.0
0.5
1.0
1.5
2.0
0 0.01 0.02 0.03 0.04
Time s
C u t t i n g f o r c e i n f e e d d i r e c t i o n N
100.0mm/min
1.0 50.010.0
Figure 10: Behavior of cutting force at various feed rates
5. Machining characteristics
5.1 Influence of the feed rate on the machined surface
The milling test was carried out at feed rates of 1.0, 10.0, 50.0 and 100.0 mm/min. The
cutting conditions for evaluation of the machining characteristics are shown in Table 3.
Cutting tests to investigate the influence of the feed rate were performed at a rotational
speed of 5000 min-1
for a depth of cut of 100 µm. Figure 10 shows the cutting force in feed
direction at each feed rate. The faster the feed rate is, the larger the cutting force. Figure 11
shows the machined surface at each feed rate.
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(a) Feed rate, 1.0mm/min
55.5 m55.5 m55.5 m
55.5 m55.5 m55.5 m 55.5 m55.5 m55.5 m
55.5
m55.5
m55.5
m
(b) Feed rate, 10.0mm/min
(c) Feed rate, 50.0mm/min (d) Feed rate, 100.0mm/min
Figure 11: Influence of feed rate on the machined surface
0.000
0.050
0.100
0.150
0.200
0.250
0.300
0.350
0.400
0.450
0.500
0 1 2 3 4 51.0 10.0 50.0 100.0Feed rate mm/min
S u r f a c e r o u g h n e s s R a
m
0.000
0.050
0.100
0.150
0.200
0.250
0.300
0.350
0.400
0.450
0.500
0 1 2 3 4 51.0 10.0 50.0 100.0Feed rate mm/min
S u r f a c e r o u g h n e s s R a
m
0.000
0.050
0.100
0.150
0.200
0.250
0.300
0.350
0.400
0.450
0.500
0 1 2 3 4 51.0 10.0 50.0 100.0Feed rate mm/min
S u r f a c e r o u g h n e s s R a
m
Figure 12: Relation between surface roughness and feed rate
While the cutting mark is confirmed on the bottom surface at the 10.0, 50.0 and 100.0
mm/min feed rates, no cutting mark is observed at the 1.0 mm/min feed rate. The cutting
mark becomes more distinct as the feed rate increases. The bottom surface roughness was
measured using the surface profiler (New View 6200, Zygo). The relation between the
surface roughness and the feed rate is shown in Fig. 12. It is clear that the surface roughnessdecreases with the feed rate.
5.2 Effect of the rotational speed on the machined surface
The milling test was also carried out at various rotational speeds of 1000, 5000, 10000 and
20000 min-1
. The feed rate and depth of cut were set to 10 mm/min and 100 µm,
respectively. Figure 13 shows the machined surface at each rotational speed. As the
rotational speed increases, the cutting marks gradually disappear. The relation between the
surface roughness and the rotational speed is shown in Fig. 14. It is clear that a high
rotational speed is appropriate in PDMS cutting.
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Journal of Advanced Mechanical Design,Systems, andManufacturing
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Vol. 2, No. 4, 2008
(a) Rotational speed,1000min-1
55.5 m55.5 m
55.5 m55.5 m 55.5 m55.5 m
55.5 m55.5 m
(b) Rotational speed, 5000min-1
(c) Rotational speed, 10000min-1 (d) Rotational speed, 20000min-1
Figure 13: Influence of rotational speed on the machined surface
0.000
0.050
0.100
0.150
0.200
0.250
0.300
0.350
0.400
0.450
0.500
0 1 2 3 4 51000 5000 10000 20000
S u r f a c e r o u g h n e s s
R a
m
Rotational speed min-1
0.000
0.050
0.100
0.150
0.200
0.250
0.300
0.350
0.400
0.450
0.500
0 1 2 3 4 51000 5000 10000 20000
S u r f a c e r o u g h n e s s
R a
m
Rotational speed min-1
0.000
0.050
0.100
0.150
0.200
0.250
0.300
0.350
0.400
0.450
0.500
0 1 2 3 4 51000 5000 10000 20000
S u r f a c e r o u g h n e s s
R a
m
Rotational speed min-1
Figure 14: Relation between surface roughness and rotational speed
5.3 Relation between the cutting depth and form of machined grooveFigure 15 shows the cutting forces in the feed direction at various depths of cut of 10, 50,
100 and 200 µm. It is clear that the deeper the cutting depth is, the larger the cutting force.
Figure 16 shows the micrograph of the cross-sectional shape and Fig.17 shows the bottom
surface roughness of the machined groove, respectively. The shapes of all the machined
grooves are precisely formed. However, for cut depths of 100 and 200 µm, the surfaces
become rough. Image measurement software (KEYENCE) was used on the micrograph
shown in Fig. 16 to measure the cutting depth and width to investigate the machining
accuracy. The results of the machined depth and width are shown in Table 4. It is clear that
the machined depth is almost the same as the desired depth, although a noticeable error of
approximately 10% is confirmed in the machined width.
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Journal of Advanced Mechanical Design,Systems, andManufacturing
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-1.5
-1.0
-0.5
0.0
0.5
1.0
1.5
0 0.01 0.02 0.03 0.04
Time s
C u t t i n g f o r c e i n f e e d d i r e c t i o n N 200µm
10100 50
-1.5
-1.0
-0.5
0.0
0.5
1.0
1.5
0 0.01 0.02 0.03 0.04
Time s
C u t t i n g f o r c e i n f e e d d i r e c t i o n N 200µm
10100 50
Figure 15: Behavior of cutting force at various depth of cuts
Table 4: Depth and width of the machined groove
Set depth m Machined depth m Machined width m
10 12.8 560.3
50 47.4 564.1
100 103.8 556.4
200 201.3 559.0
(a) 10 m depth
66.6 m66.6 m
66.6 m66.6 m 66.6 m66.6 m
66.6 m66.6 m
(b) 50 m depth
(c) 100 m depth (d) 200 m depth
Figure 16: Cross-sectional view of the machined groove
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0.000
0.050
0.100
0.150
0.2000.250
0.300
0.350
0.400
0.450
0.500
0 1 2 3 4 510 50 100 200
Depth of cut µm
S u r f a c e r o u g h n e s s R a
m
0.000
0.050
0.100
0.150
0.2000.250
0.300
0.350
0.400
0.450
0.500
0 1 2 3 4 510 50 100 200
Depth of cut µm
S u r f a c e r o u g h n e s s R a
m
0.000
0.050
0.100
0.150
0.2000.250
0.300
0.350
0.400
0.450
0.500
0 1 2 3 4 510 50 100 200
Depth of cut µm
S u r f a c e r o u g h n e s s R a
m
Figure 17: Relation between surface roughness and depth of cut
6. Conclusion
Cryogenic micro milling of PDMS is proposed for the fabrication of microfluidic chips. A
special jig with a liquid nitrogen chamber was developed as the cooling system for
cryogenic machining. The validity of the proposed milling technology was evaluated by
several cutting tests. The results are summarized as follows.
1) With cryogenic cooling, PDMS can be machined and a micro groove can be shaped
precisely. The machining process works on PDMS at temperatures below the glass
transition temperature.
2) Under the cutting condition of a lower feed rate, cutting marks disappear and the
machined surface becomes fine. Especially at a feed rate of 1.0 mm/min, the machined
surface roughness achieves Ra=80 nm.
3) When the rotational speed is higher and the depth of cut is smaller, the machined surface
is also improved.
Since PDMS has the lowest glass transition temperature of polymer materials, it is
suggested that the cryogenic cutting process with liquid nitrogen will also be useful for
micromachining of other elastic polymer materials.
Acknowledgement
The machining center used in the research has been provided by Machine Tool
Technologies Research Foundation (MTTRF) and a part of this research is supported by
Machine Tool Engineering Foundation. Authors would like to express our appreciation for
these supports.
References
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(2) Bundgaard F. et al., Rapid Prototyping Methods for All-COC/Topas Waveguides and
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(3) Yokota K., An Introduction to Polymer materials, KAGAKU-DOJIN PUBLISHING
CO. 1999, pp. 95-101, 143-161.
(4) Hira S., Micro-cutting of Polytetrafluoroetylene (PTFE) for Application of
Micro-Fluidic Device, Key Eng Mater, Vol.329, (2006), pp. 577-582.
(5) Matsumura T., Machining System for Micro Fabrication on Glass, Proceedings of 2004
JUSFA, (2004), pp. 1-6.