Download as pdf or txt
Download as pdf or txt
You are on page 1of 6

Optical and Mechanical Properties of a Polyimide Membrane

for Tunable Lenses


Christian Kelba , Dominik Hoheiselb , Eduard Reithmeiera , Lutz Rissingb
a Hanover Center of Optical Technologies, Nienburger Straße 17, 30167 Hannover, Germany;
b Institute for MicroProduction Technology, An der Universtität 2, 30823 Garbsen, Germany

ABSTRACT
With its chemical resistance and easy structurability, polyimide (PI) makes for a fine candidate for membranes
of tuneable optical systems. Disadvantages of the material are its high absorption coefficient and its mechanical
stability, which prevents high deflections of the membrane. To improve the optical capabilities of the material,
different variations of processing of the membrane are used.
For fabrication of the PI membrane, a photosensitive PI precursor is used. The precursor is spin coated on a
4”’ Si wafer. After a prebake, the wafer is exposed to UV light. To manipulate the optical properties, different
types of postbake are investigated. Afterwards, the backside of the wafer is structured by Deep Reactive Ion
Etching (DRIE). Thus, a temporary photoresist etching mask is manufactured by photolithography on the wafer
backside. Circular structures with a diameter of 2 mm are then etched through the wafer to fabricate the
membranes.
The absorption coefficient of the different manufactured membranes is measured. For future use of the
membrane as part of a variable optical system, a FEM-Model is built to predict the behaviour of the membrane
under mechanical loads, especially considering strains and stresses induced by the different postbake types. The
results of the FEM-Model are compared with experimental data obtained via digital image processing methods.
Comparative data using different membrane materials are also presented to compare the performance of the PI
membrane.
Keywords: polyimide, membrane lens, tunable lens

1. INTRODUCTION
During the last years, the research on tunable single-lens systems covered a vast amount of different actuation
technologies like e.g. electrowetting,1 heat expansion of optic fluids,2 piezo-active materials3 and some more,
see also a review by Nguyen.4 Apart from electrowetting, most systems that are using these technologies
use polydimethylsiloxan (PDMS) as membrane material to cover the lens-fluids that are otherwise subject to
evaporation or contamination by other substances. To produce this membranes, PDMS-solution can be applied
on a Si-Wafer via spincoating and then cured. The PDMS sticks to the Si-wafer because of adhesion and the
membranes can be manufactured by removal of the Si by e.g. deep reactive ion beam etching (DRIE).
While according to Mukhopadhyay5 the production of PDMS membranes can be done time efficiently and
with low cost and their optical capabilities are well suited for optical applications, they also manifest drawbacks
like fast change of their mechanical properties due to aging or the change of characteristics by absorption of
molecules they are in contact with. The first issue can cause a bad predictability of membrane behaviour with
respect to a control parameter such as pressure, since the membrane behaviour is mostly analysed by beforehand
simulations6 or measurement of focal length on the real system.7 The second issue can cause a change of optical
properties by e.g. absorpiton of fluorescent molecules.5
Therefore, as alternative system to PDMS, we chose to study Polyimide (PI), because its processing charac-
teristics are well-known from the use of PI as a sacrificial or functional layer in microelectromechanical systems
For further information contact Christian Kelb:
E-Mail: christian.kelb@hot.uni-hannover.de
Telephone: +49 (0)511 762-17943

Polymer Optics and Molded Glass Optics: Design, Fabrication, and Materials II, edited by David H. Krevor, William S. Beich,
Michael P. Schaub, Stefan M. Bäumer, Proc. of SPIE Vol. 8489, 84890F · © 2012 SPIE · CCC code: 0277-786/12/$18
doi: 10.1117/12.929773

Proc. of SPIE Vol. 8489 84890F-1

Downloaded From: http://proceedings.spiedigitallibrary.org/ on 09/21/2013 Terms of Use: http://spiedl.org/terms


a) e)

b) 55555 AM.
f) 555555
c)

d) h)

Si AZ® 9260 i)
PI Mask

UV-light i)

Figure 1. Fabrication process of the PI membrane: a) spin coating PI precusor; b) prebake; c) flood exposure; d) postbake;
backside processing: e) spin coating AZ R 9260; f) softbake; g) exposuring; h) patterning by developing; i) deep reactive
ion etching; j) stripping AZ and dicing.

(MEMS).8 PI-Membranes can be produced similar to PDMS-Membrane by applying a PI-solution to a Si wafer


by spincoating, followed by a post-bake to trigger cross-linking of the material. The mechanical resistance of
PI allows the processing of thinner membranes (see section 2) and its chemical resistance8 allows application of
PI-membranes in more agressive media.

2. PRODUCTION OF THE MEMBRANES


For fabrication of a polyimide (PI) membrane, a photosensitive polyimide precursor (Durimide R
from Fuji) is
used. A 4” Si wafer, polished from both sides, is utilized as a substrate. In a first step, the substrate is cleaned
and afterwards it is dehydrogenised on a hot plate. After a rapid cooling step, the precursor is applied to the
substrate with a spin coater RC8 from SÜSS MicroTec. After a relaxation time, the precursor is prebaked on
a hot plate to evaporate the solvent. The next step is to expose the precursor using ultraviolet (UV) light
in a mask aligner MA6/BA6 from SÜSS MicroTec. As there is no need to pattern the membrane, a flood
exposure is applied. For a patterned polyimide film, an exposure through a mask and a development with the
developer/ rinser combination QZ3501/ QZ3512 would be necessary. In order to achieve a manipulation of the
optical properties, two types of postbake are investigated. Firstly, postbake in an electric heater at 360 ◦ C under
N2-atmospere; secondly, postbake in a vacuum oven at 360 ◦ C.
After the postbake, the backside of the wafer is patterned by Deep Reactive Ion Etching (DRIE) to fabricate
membranes. Therefore, the positive photoresist AZ 9260 is spin coated on the backside of the substrate. After
a soft bake, the backside of the wafer is exposed to UV light through a mask with circular structures with a
diameter of 2 mm. The exposed areas of the photoresist become developable to the developer AZ 400K. In this
way, a temporary photoresist etching mask is manufactured by photolithography on the wafer backside. For
generating the membranes, the backside of the wafer is etched by DRIE. This etching process is also known as
Bosch-process and consists of two alternating steps. The first step is an isotropic etching by ions from a plasma
and the second step is deposition of a polymer passivation layer to shield the side walls from etching. Altogether,
an anisotropic etching of silicon can be obtained.9 By this, membranes made of PI with a diameter of 2 mm are
manufactured on a silicon frame. The process is shown in order in figure 1.
After the fabrication of the membranes, the samples featured a thickness of about 5 µm, determined by the
spin-coating process of the durimide precursor. For further thinning, the membranes were treated in a plasma
asher, until the first membranes completely dissolved. Afterwards, the membranes were seperated by dicing and

Proc. of SPIE Vol. 8489 84890F-2

Downloaded From: http://proceedings.spiedigitallibrary.org/ on 09/21/2013 Terms of Use: http://spiedl.org/terms


a) b) 60

50

40

intensity
30

20

10

0
0 0.5 1 1.5 2 2.5 3
1mm
vertical position in µm

Figure 2. a) photograph of the PI-membrane on the Si-Chip mounted on a PMMA-substrate for measurement purposes,
b) intensity curves obtained by measurements with a confocal microscope showing peaks from each membrane boundary

mounted on a PMMA-carrier for testing purposes. Figure 2 a) shows the mounted membrane in a close-up.
On inspection using a microscope it was found that some membranes showed concentric circular structures and
leftover chips from the abrasive cutting second of which could be removed by simple washing of the membranes.

3. MEASUREMENT AND SIMULATION OF MECHANICAL PROPERTIES


To determine the mechanical properties of the membranes, measurements of the thickness and of the deflection
behavior were done. The measurement of the membrane thickness was done by recording confocal curves of the
samples with a Nanofocus µSurf confocal microscope. The results of a measurement of three points on the same
membrane are shown in figure 2 b) where the peaks mark the position of the two membrane surfaces.
The distance between the peaks equals the optical pathlength between the two membrane surfaces and can
be converted to the mechanical pathlength by dividing with the refractive index n, which is assumed as n = 1.70
as written in Dupont’s summary of properties for kapton film.10 The measured optical pathlength differed
between 839 nm and 545 nm which results in membrane thicknesses of 494 nm down to 315 nm. The recorded
length was achieved by calculating a median value of points on the membrane, where a clean confocal curve with
two peaks could be found. Although results of this measurements are influenced by aberrations caused by the
polyimide layer (similar to measurements through cover glass where corrected objective lenses are available for)
the induced errors are neglectable for thin parallel layers according to Cox’ work on measuring thin layers by
confocal microscopy.11
As can be seen in figure 2 b), the distance between the peaks hits the vertical resolution of the confocal
microscope, causing the two seperate peaks drifting together. On several places on the membrane a differentiation
between the two peaks was not possible. Besides limitations through lower resolution, this can be explained by
a partial lower transmittance of the membrane and accordingly a higher damping of the second peak, causing it
to merge with the peak from the upper boundary. For thickness measurements that are more precise, reflection
coating of the membrane backside could be of use.
For future use of the membrane in a membrane-covered lens a number of tests were conducted in which the
deflection of the membrane was measured if pressurized from 0 to 2 kPa. Here, the deflection was measured by
a Keyence confocal line scanner with a scan width of 1100 µm, a lateral resolution of 2 µm and a resolution of
10 nm in vertical direction. The results of these experiments are shown in figure 3 as a plot of the maximum
deflection (i.e. on top of the membrane) with respect to pressure. The membrane deflection shows a strongly
non-linear behaviour, but does not correlate with the membrane thickness as measured. Here, a reduction of the
maximum deflection with increasing membrane thickness was to expect. An explanation can be found in the
differing effects of the DRIE-thinning process on the membranes, that is already observable in the also differing
membrane thicknesses; It is possible, that the etching process for thinning also influenced the Young’s modulus

Proc. of SPIE Vol. 8489 84890F-3

Downloaded From: http://proceedings.spiedigitallibrary.org/ on 09/21/2013 Terms of Use: http://spiedl.org/terms


t = 315nm
t = 369nm
max deflection in µm
t = 444nm
t = 473nm
t = 476nm
t = 494nm

pressure in kPa
Figure 3. Results of deflection measurements of the produced membranes.

or the inital strain of the membrane. Defects in membrane thickness like areas of significantly lower thickness
that can not be measured by the confocal microscope can also contribute to greater flexibility.
It should be mentioned that the linear deflection at a pressure of about 1 kPa occurs, because plastic de-
formation starts to add to the elastic deformation and therefore makes the deformation process irreversible.
Several membranes were tested for plastic deformation up to a pressure of about 4 kPa without failure but were
permanently deformed which could still be observed weeks after the deflection experiments. In future research,
a controlled plastic deformation of the membranes could be used to handle initial strain or to set another focal
length as infitiy (i.e. the membrane is a flat surface) in inactive state.
To predict the deflection of the membranes to a certain precision, a simple FEM-model was built using
COMSOL with special attention to model nonlinear deflection behaviour. The use of a viscoelastic model for
material behaviour yielded similar results to the measurements taken beforhand. The material properties were
set to a Young’s modulus of E = 2.5 GPa an a Poisson’s ratio of 0.35 as can be found in the datasheet of the used
polyimide.12 To model a shrinking of the PI during the postbake, a inital radial stress of 10 kPa was set. As can
be seen in 4, the results show the same qualitative behaviour as the results of the measurement. Although the
deflection is getting smaller with increasing membrane thickness, the differences are relatively small compared
to the change in membrane thickness of about 66 %. The small depence of membrane deflection from thickness
in the simulation can explain the observed independence between membrane thickness and deflection in the
measurements. A change of the material properties or intial stress by the DRIE-etching-process can therefore
have a bigger effect on deflection behaviour than the difference in membrane thickness.
A second simulation was done with a constant membrane thickness of the maximum deflection from membrane
thickness can be caused by the already discussed variance in Young’s modulus.

4. TRANSMISSION SPECTRUM
As mentioned in section 2, the membranes where treated by postbake-processes under N2 -atmosphere and in
vacuum. Figure 5 shows the results of the different treatments in a transmission spectrum between 190 nm and
900 nm. The measurements were taken with a Kontron Uvikon 9300 spectrometer which provides a spectral
resolution of 1 nm. For comparison purposes the transmission spectra of a PDMS and a PMMA layer with
varying thickness are shown as well. Both membranes were manufactured only by spincoating without the
etching process for thinning. Although the membranes posses the same thickness of 5 µm, the membrane which
was postbaked in vacuum shows a significantly higher transmission as the membrane, that was postbaked in
N2-atmosphere.
Although the transmission of both PI-membranes is not as high as the transmission trough the much thicker
comparion samples, the measurement shows that the transmission could be tuned by variation of the postbake

Proc. of SPIE Vol. 8489 84890F-4

Downloaded From: http://proceedings.spiedigitallibrary.org/ on 09/21/2013 Terms of Use: http://spiedl.org/terms


a)
100
80
deflection in µm

60
Young’s modulus = 2.00GPa
Young’s modulus = 2.25GPa
40
Young’s modulus = 2.50GPa
20 Young’s modulus = 2.75GPa
Young’s modulus = 3.00GPa
0
0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 2
b) pressure in kPa
100
80
deflection in µm

60 t = 300nm
t = 350nm
40
t = 400nm
t = 450nm
20
t = 500nm
0
0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 2
pressure in kPa
Figure 4. a) Simulation results of a FEM-Simulation of the deflection under pressure for varying Young’s moduli and a
membrane thickness of 400 nm b) Simulation results of a FEM-simulation of the pressurized membranes deflection with
varying thicknesses and a Young’s modulus of 2.5 GPa

100
transmission in percent

80

60

40
PDMS, 1mm
polyimide, 5µm, N²
20 polyimide, 5µm, vacuum
PMAA, 5mm
0
100 200 300 400 500 600 700 800 900
wavelength in nm
Figure 5. Transmission spectra of different processed polyimide membranes in comparison to other materials

Proc. of SPIE Vol. 8489 84890F-5

Downloaded From: http://proceedings.spiedigitallibrary.org/ on 09/21/2013 Terms of Use: http://spiedl.org/terms


process to a point, were it reaches the transmission of the PMMA sample at 900 nm wavelength. Therefore, the
membranes are interesting for optical applications with wavelength above 700 nm.

5. CONCLUSION
In this paper, we were able to show in a proof-of-concept, that it is possible to produce membranes with at
least average optical capabilities starting from a polyimide precursor for photostructuring. The original intended
minimal thickness of 5 µm achievable by spincoating could be reduced by a factor of more than 10 to under
400nm by DRI-etching which is already a well-known process in processing microelectronics and micromechanics.
The optical capabilities of this precursor could be tuned by a postbake process in vacuum to a state where it
can be used as a lens for wavelengths of about 900 nm.
Although the deflection behaviour of the membrane can not be predicted completely by knowledge of only the
membrane thickness, it was possible to find a material model which fits the qualitative behaviour of deflection
under pressure to a certain point. This provides the basis for a future simulation of lenses fitted with the shown
membrane type. Altough, a method for measuring Young’s moduli simulatiously with initial stresses has to be
applied in order the improve the precision of the simulations. Alternatively, the production has to be stabilized
to a point where the membranes behave similar, so that material constants and initial strains and stresses can
be determined by a fit of the viscoelastic material model.
Alltogether, the chemical and mechanical stability of PI together with the possibility to alter its optical
and mechanical properties by means of processes already used in production of microsystems can make it to a
competitor for the commonly used PDMS as membrane material. This applies especially for the use in the wave-
length region of above 700 nm. Future research will center on a better control of membrane thickness and surface
quality by the plasma ashing process. Then, a fit of the viscoelastic material model could succeed in determining
Young’s modulus and initial stress of the membrane for better prediction of membrane movement. Finally an
investigation of the membrane transmission spectre in NIR-wavelengths (i.e. above 900 nm up to 2000 nm) could
be conducted. This would help in determining the applicability of the membranes in biotechnologies.

REFERENCES
[1] Krogmann, F., Monch, W., and Zappe, H., “Electrowetting for tunable microoptics,” Journal of Microelec-
tromechanical Systems 17(6), 1501–1512 (2008).
[2] Lee, S.-y., Tung, H.-w., Chen, W.-c., and Fang, W., “Thermal actuated solid tunable lens,” IEEE Photonics
Technology Letters 18(21), 2191–2193 (2006).
[3] Kaneko, T., Ohmi, T., Ohya, N., Kawahara, N., and Hattori, T., “A new, compact and quick-response
dynamic focusing lens,” Proceedings of 1997 International Conference on Solid State Sensors and Actuators
, 63–66 (1997).
[4] Nguyen, N.-T., “Micro-optofluidic lenses: A review,” Biomicrofluidics 4(3), 031501 (2010).
[5] Mukhopadhyay, R., “When pdms isn’t the best,” Analytical Chemistry 79(9), 3248–3253 (2007).
[6] Werber, A. and Zappe, H., “Tunable microfluidic microlenses,” Applied Optics 44(16), 3238 (2005).
[7] Wang, W. and Fang, J., “Design, fabrication and testing of a micromachined integrated tunable microlens,”
Journal of Micromechanics and Microengineering 16(7), 1221–1226 (2006).
[8] Wilson, W. C. and Atkinson, G. M., “Review of polyimides used in the manufacturing of micro systems,”
(2007).
[9] Ayón, A., Zhang, X., and Khanna, R., “Anisotropic silicon trenches 300–500 µm deep employing time
multiplexed deep etching (tmde),” Sensors and Actuators A: Physical 91(3), 381–385 (2001).
[10] Blair, K., “Summary of properties for kapton polyimide films.”
http://www2.dupont.com/Kapton/en US/assets/downloads/pdf/summaryofprop.pdf. online, accessed
13-July-2012.
[11] Cox, G. and Sheppard, C. J., “Measurement of thin coatings in the confocal microscope,” Micron 32(7),
701–705 (2001).
[12] De Cauwer, I., “Technical product information on durimide 7300 photosensitive polyimide precursor.”
http://www.fujifilmusa.com/shared/bin/Durimide 7300 US12.pdf (2012). online, accessed 13-July-2012.

Proc. of SPIE Vol. 8489 84890F-6

Downloaded From: http://proceedings.spiedigitallibrary.org/ on 09/21/2013 Terms of Use: http://spiedl.org/terms

You might also like