Journal of Advanced Mechanical Design,

Systems, and
Manufacturing

Vol. 2, No. 4, 2008

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: kakinuma@sd.keio.ac.jp

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 for
rapid 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, -TAS, Microfluidic
Chip

1. Introduction

*Received 21 Mar., 2008 (No. 08-0205)

[DOI: 10.1299/jamdsm.2.560]

Recently, the study of -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 -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 -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

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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.
Si

Patterning photoresist
(Si Mold)

Si plate
Photoresist coating

PDMS

Thermosetting PDMS
Mask

Development

Micro groove formed

Figure 1: Multi process of photolithography

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 196C. 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-transition
temperature centigrade
Polydimethylsiloxane
-123
Polyethylene
-30
Polypropylene
-10
Polymethylmethacrylate
105
Polycarbonate
150
Nylon 66
60
CH3
CH2

CH3

C=O

Si

CH3

CH3
(a) PMMA

(b) PDMS

Figure 2: Molecular structure of PMMA and PDMS

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3. Applying cryogenic cooling to the cutting process

Vol. 2, No. 4, 2008

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 room
temperature 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.
100
Hardness (JIS K 6253 TypeA)

90
80
70
60
50
40
30
20
10
0

PDMS at

room temperature

PDMS at
PMMA at

ultralow temperature room temperature

Figure 3: Hardness of the PDMS at room temperature and at ultralow temperature

: Temperature-measured point

Liquid nitrogen

End mill
PDMS
Workpiece holder
Liquid nitrogen
chamber

60mm

Bakelite flame

110mm

Dynamometer

Water circulation
system

Table

Figure 4: Structure of cryogenic jig

Micro square end mill
PDMS

Cryogenic cooling fixture

Water

Figure 5: Appearance of cryogenic machining system

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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 the
reservoir 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 -170C and -196C. 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 -196C. 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
-170C.
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.
50

Under the water circulation system

0
Temperature

500

1000

1500

2000

2500

3000

-50

Aluminum
-100

Machining space

-150

PDMS surface

-200
Adding the liquid nitrogen

No liquid nitrogen

Time s

Figure 6: Temperature property of the cryogenic jig

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 angle
of 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 500m 700m.

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Table 2: Cutting condition of PDMS at room temperature and at ultralow temperature

Rotational speed
5000min-1
10.0mm/min
Feed rate
Feed per tooth
1.0m
Micro square end mill
Tool
Diameter of tool
0.5mm
PDMS
Workpiece
3-axis vertical type
Machine tool

100m

66.6m

(a) Side view

(b) Bottom of edge

Figure 7: Micro square end mill (0.5)

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 m and the depth is approximately 200 m. The desired shape is
500 m wide and 200 m 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 20m in this test, measured statically by dial gauge with resolution of
1m. Therefore, it is necessary to suppress the tool runout and consider the difference of
shrinkage between tool and workpiece for accurate machining.
1.0

1 revolution

Cutting force in feed direction N

0.8

At ultralow temperature
At room temperature

0.6
0.4
0.2
0.0
-0.2

0.01

0.02

0.03

0.04

0.05

-0.4
-0.6
-0.8
Time s

Figure 8: Cutting force at room temperature and ultralow temperature

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100m

100m
Top view

Top view

100m
Side view
(a) At room temperature

66.6m
Side view
(b) At ultralow temperature

Figure 9: Shape of machined groove (PDMS)

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 m. 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.
Table 3: Cutting condition for evaluation of machining characteristics
at room temperature and at ultralow temperature
Feed rate change
Rotational speed change
depth change
5000min-1
5000min-1
Rotational speed
1000,5000,10000,20000min-1
Feed rate
1.0,10.0,50.0,100.0mm/min
10.0mm/min
10.0mm/min
Feed per tooth
0.1, 1.0, 5.0, 10.0m
5.0, 1.0, 0.5, 0.25m
1.0m
Depth of cut
100m
100m
10,50,100,200m
Tool
Micro square end mill
Diameter of tool
0.5mm
Workpiece
PDMS
Machine tool
3-axis vertical machining center

Cutting force in feed direction N

2.0

100.0mm/min

1.5

10.0
1.0

1.0

50.0

0.5
0.0
-0.5

0.01

0.02

0.03

0.04

-1.0
-1.5
-2.0

Time s

Figure 10: Behavior of cutting force at various feed rates

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55.5m

55.5m
(a) Feed rate, 1.0mm/min

(b) Feed rate, 10.0mm/min

55.5m
(c) Feed rate, 50.0mm/min

55.5m
(d) Feed rate, 100.0mm/min

Figure 11: Influence of feed rate on the machined surface

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 roughness
decreases with the feed rate.

Surface roughness Ra m

0.500
0.450
0.400
0.350
0.300
0.250
0.200
0.150
0.100
0.050
0.000
0

1.0
1

10.0
50.0
2
3
Feed rate mm/min

100.0
4

Figure 12: Relation between surface roughness and 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 m,
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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55.5m

55.5m
(a) Rotational speed,1000min-1

(b) Rotational speed, 5000min-1

55.5m

55.5m

(c) Rotational speed, 10000min-1

(d) Rotational speed, 20000min-1

Figure 13: Influence of rotational speed on the machined surface

0.500

Surface roughness Ra m

0.450
0.400
0.350
0.300
0.250
0.200
0.150
0.100
0.050
0.000
0

1000
1

5000
10000
2
3
Rotational speed min-1

20000
4

Figure 14: Relation between surface roughness and rotational speed

5.3 Relation between the cutting depth and form of machined groove
Figure 15 shows the cutting forces in the feed direction at various depths of cut of 10, 50,
100 and 200 m. 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 m, 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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Cutting force in feed direction N

1.5

200m

1.0

100

10

0.5

50

0.0
0

0.01

0.02

0.03

0.04

-0.5
-1.0
-1.5
Time s

Figure 15: Behavior of cutting force at various depth of cuts

Table 4: Depth and width of the machined groove

Set depth m
10
50
100
200

Machined depth m
12.8
47.4
103.8
201.3

66.6m
(a) 10m depth

66.6m
(c) 100m depth

Machined width m
560.3
564.1
556.4
559.0

66.6m
(b) 50m depth

66.6m
(d) 200m depth

Figure 16: Cross-sectional view of the machined groove

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0.500

Surface roughness Ra m

0.450
0.400
0.350
0.300
0.250
0.200
0.150
0.100
0.050
0.000
0

10
1

50
100
2
3
Depth of cut m

200
4

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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Micro-Channels in SU8, Proceedings of 9th International Conference of Miniaturized
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(2) Bundgaard F. et al., Rapid Prototyping Methods for All-COC/Topas Waveguides and
Microfluidic Systems, Proceedings of 9th International Conference of Miniaturized
Systems for Chemistry and Life Sciences, (2005) pp. 1200-1202.
(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.
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