Partially athermalized waveguide gratings

Muhammad Rizwan Saleem a,b,*, Seppo Honkanen a, Jari Turunen a

a
University of Eastern Finland, Department of Physics and Mathematics, P. O. Box 111, FIN-80101
Joensuu, Finland
b
National University of Sciences and Technology (NUST), School of Chemical and Materials
Engineering (SCME), Sector H-12, Islamabad, Pakistan
* Corresponding author: (Tel) +358 50 442 3469, (Fax) +358 13 251 3290
E-mail: rizwan.saleem@uef.fi

ABSTRACT

We investigated high efficiency organic-inorganic hybrid sub-wavelength binary diffraction gratings as partially
athermalized waveguides. The performance of the grating is evaluated in terms of low spectral shifts in heating
environment. The efficiency was determined to be least effective in temperature environment around room temperature.
The spectral characteristics of waveguide remain thermally stable by selecting optical grade polymer materials with high
thermal expansion coefficients, subsequently deposited by high index, amorphous TiO2 thin films by atomic layer
deposition (ALD) process. The spectral shifts towards longer and shorter wavelengths were investigated in terms of two
main parameters, thermal expansion coefficient (TEC) and thermo-optic coefficient (TOC) respectively. Realization of
partially athermalized waveguides are described by complete agreement in theoretically calculated and experimentally
measured results in the temperature range of 100 °C.
Key words: Diffraction grating, Optical materials, Atomic layer deposition, thermo-optic coefficient

1. INTRODUCTION
Advances in diffractive optics have made design, analysis and fabrication of diffractive optical elements (DOEs) with
sub-wavelength grating structures an attractive choice for various applications in polymer optical materials1. DOEs
shows guided mode resonance phenomena for incident electromagnetic waves over a selectable parameter range for
smart device applications2. Transparent polymers have gained increased importance in diffractive optics over the last
decade3. Polymeric (organic) optical devices have advantages over inorganic devices in several applications4. For
example, inorganic glasses are less flexible, more brittle and require higher processing temperatures; in addition, they
also require some sophisticated etching techniques for the fabrications of nano-patterns on substrates. On the other hand,
polymer based optical components can be fabricated, for example, simply by replicating the structures from
corresponding master stamp (usually at relatively low processing temperatures) and thus overcome some of the
disadvantages of inorganic glasses. The use of polymers, such as polycarbonate, polymethyl methacrylate, polystyrene
and polycyclohexyl methacrylate exhibit coefficients of thermal expansion nearly ten times than those of optical glasses5.
The values of coefficient of thermal expansion and thermo-optic coefficients for polycarbonate calculated by several
researchers are nearly 6.55 x 10-5 and -1.07 x 10-4 °C-1 respectively6,7 in presence of some useful analytical relations
between two parameters at various temperatures ranges8. The use of inherent thermal expansions of polymers were
exploited to shift central resonance peak to longer wavelengths which may also be attributed as an increase in periodicity
of binary gratings. Refractive index variations of amorphous polycarbonate with temperature follow Lorentz-Lorenz law
without undergoing transitions. These refractive index variations of polymers are attributed to changes in the coefficient
of thermal expansions and consequently to a change in density of respective material9. Most economic sub-micron
diffraction grating structures in organic materials can be generated by employing efficient replication of standard high
pressure heating tool techniques such as injection molding, hot embossing10. Hot embossing is a two-step compression
molding cycle in which already formed thin polymer film is heated through conduction near its transition temperature
and then filling of the microcavities by compression in second step11.
Amorphous TiO2 films deposited by atomic layer deposition ALD is a high refractive index and transparent material
to entire visible range. ALD is a modified form of chemical vapor deposition CVD in which film grows by means of a
cyclic process through a series of surface reactions between the adsorbing precursor species and already left over reactive

Micro-Optics 2012, edited by Hugo Thienpont, Jürgen Mohr, Hans Zappe, Hirochika Nakajima,
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precursor species by previous pulse12. Thin TiO2 films deposited by ALD distinguish it from other deposition techniques
in terms of atomic level thickness, composition, large area uniformity, thermal decomposition and film conformality
control. Amorphous TiO2 films grown by ALD have been successfully employed for the coupling of externally
propagated light into a waveguide mode of resonant waveguide grating structures on glass and silicon substrates13. The
refractive index decreases with temperature rise which is described due to density changes in the material. Thermo-optic
coefficient dn/dT of evaporated TiO2 films on cleaved fibers was reported to decrease with temperature rise and
extremely sensitive to environmental effects14. The performance and operation of optical devices composed of TiO2
coatings are greatly influenced under various environmental conditions15. DOE’s can be incorporated with optical system
to monitor and tailor the properties under various environmental conditions. In addition, polymeric optical devices are
more sensitive to environmental changes such as temperature and humidity and undergo physical changes in their
performance which may be attributed to variation in their respective thermal expansion and thermo-optic coefficients16.
A combined effect responsible for these individual factors of dimensional and index changes would lead to
athermalization of overall behavior of optical systems17. Figure 1 shows a binary, planar and unslanted diffraction
grating profile with a magnified view as a result of thermal expansion of polycarbonate substrate coated by TiO2
amorphous cover layer and then exposed by plane waves at desired angle of incidence.

Figure 1. Binary, planar, and unslanted diffraction grating on polycarbonate substrate coated by TiO2 amorphous cover layer with
an expanded grating profile’s view due to thermal expansion.

The purpose of this paper is to show the effect of temperature changes on the position of central resonance
wavelength. For this purpose we investigate the effect of various grating geometrical parameters on the thermal
properties of polymer guided mode resonance filters. Since, polymer materials are sensitive to thermal changes and result
in variations of optically coupled field due to change in geometrical parameters of grating such as interfacial profile,
grating period, grating height, and fill factor. In particular, the influences of two major factors contributing towards the
shift of the center resonance wavelength are in general, thermal expansion and thermo optic coefficient of the polymer
and dielectric materials. The use of high thermal expansion polymeric materials to investigate the center wavelength shift
clearly demonstrated an improvement in the thermal sensitivity of fiber Bragg gratings for temperature sensing
purposes18. On the other hand, polymer materials such as polycarbonate and thin dielectric films like TiO2 have negative
thermo-optic coefficients and can be used for partially thermally stabilized optical devices.

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 2. EXPERIMENTAL
The experimental part consists of structure fabrication and replication, structure and optical characterization.
2.1 Structure fabrication and replication
Silicon wafer with <100> crystal orientation, 2˝ in diameter were spin coated by a high resolution negative
binary tone resist HSQ XR-1541 from Dow Corning with constituents isobutyl methyl ketone, hydrogen silsesquioxane
and toluene. The RPM and time of spin coating was adjusted to get targeted film thickness of ~120 nm which was the
desired height of grating structure. The HSQ film thickness was measured by Dektak 150 stylus surface profilometer
manufactured by Veeco Metrology. Electron beam Lithographic patterns were written on HSQ resist at an area of 25
mm2 by Vistec EBPG5000+ES HR electron beam pattering tool at a scaled dose of 6000µC/cm2. After exposure, the
resist was developed with MP 351 developer which contains disodium tetraborate decahydrate and sodium hydroxide
and water solution with the ratio 1:3 followed by rinsing with isopropanol and water for 90 and 30 seconds respectively.
After development, sample was heat treated for 3 hours at a temperature of 300 °C in an oven. The heat treatment
process transforms HSQ as a hard material with similar properties to silica as a stamping hard material. The heat treated
sample was then subjected to surface treatment to deposit a silane layer with silanization solution composed of a mixture
of HFE 7100 engineering solvent with 0.2% of trimethylhydroxysilane (TMS) in presence of nitrogen atmosphere to act
as a de-adhesive layer when stamped into polycarbonate substrate. Polycarbonate sheets were purchased from
Makrofol® DE PC film in the form of thin films of ~170 µm thickness. The replication was performed by using Obducat
Eitre® 3 imprinter. Replication process needs to heat the stamp at a temperature of 165 °C, slightly above the glass
transition temperature of polycarbonate, and then a pressure of 50 bar was applied for 2 minutes and finally 100 % air
cooling was applied19. Replication was followed by a thin film deposition (61 nm) of amorphous TiO2 by using Beneq
TFS 500 ALD reactor at a deposition temperature of 120 °C with commonly known precursor TiCl4 and H2O materials.
2.2 Structure and optical characterization

Structural characterization is performed by scanning electron microscope (SEM LEO 1550 Gemini). Optical
properties of thermal grating structures are characterized by a variable angle spectroscopic ellipsometer VASE
manufactured by J. A. Woollam Co. Ellipsometer is employed to measure the spectral reflectance resonance for TE-
Mode at an incident angle of 20° with normal to the grating in the wavelength range 750–880 nm with beam spot size of
3 mm. The polycarbonate grating was placed firmly against a home-built aluminum hot plate whose temperature was
controlled and monitored carefully. The heating rate was 0.5 °C/min with an accuracy of ±0.1 during each measurement
interval. The surface of aluminum hot plate was rubbed with a fine sand paper to eliminate any back reflections. Each
thermal spectral measurement is performed by a temperature interval of 5 °C, the material may be considered at thermal
equilibrium at each temperature interval. The refractive index measurements of ALD coated TiO2 films were also
measured at various temperatures by ellipsometer and then employed directly into calculations to observe the behavior of
central resonance wavelength shift.

3. DESIGN OF WAVEGUIDE GRATINGS WITH SIMULATION RESULTS

Fourier Modal Method (FMM) based on rigorous diffraction theory is applied for the design of binary, planar,
unslanted and asymmetric (different refractive indices on both sides of structure) diffraction grating in polycarbonate
substrate are shown in Fig. 1 with the following parameters; period d=425 nm, fill factor f =0.63, structure height h=120
nm, TiO2 thickness t=61 nm, incidence angle θi=20°, and central resonance wavelength λr=855 nm. The refractive
indices of air, TiO2 and polycarbonate are n1=1, n2=2.3224, and n3=1.58 at resonance wavelength respectively.
In figure 2a, h is calculated as a function of t to give maximum diffraction efficiency at the resonance condition. In
order to attain maximum efficiency the increase in h is compensated by a reduction in t. Since ALD coated films are
much more precise due to atomic level deposition and it acts as an independent process with respect to fabrication. This
means that any changes in the desired profile (h) during fabrication process can be compensated by ALD cover layer
thickness t to maintain maximum efficiency of designed structure. Figure 2b shows grating fundamental behavior in
terms of variation in resonance wavelength with respect to incidence angle (the angle between the incident light and
grating normal) keeping all other design fixed parameters; it demonstrates grating behavior before subjecting to thermal
changes. Fig. 2c illustrates very interesting result between h and f. The increase in h is compensated by a reduction in f of
the same profile in order to fulfill the maximum efficiency condition by keeping the overall area of diffracting pattern

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nearly constant. Figure 2d shows the limitations over variations of refractive indices of both the materials (substrate and
cover layer).
(a) (b)
TE-Mode reflectance resonance Resonance wavelength and angle of incidence
66 25
0.9 24 0.9

64 0.8 23 0.8

Incident Angle θi [degree]

TiO 2 film thickness [nm]

X: 120, Y: 61
0.7 0.7
Index: 1 22
62 0.6 X: 855, Y: 20 0.6
21 Index: 1
0.5 0.5
20
60 0.4 0.4
19
0.3 0.3
58 18
0.2 0.2
0.1 17 0.1
56 16
115 120 125 850 852 854 856 858 860
Grating ridge height [nm] Wavelength λ [nm]

(c) (d)
Relation between grating structure height and fill factor Refractive indices of Polycarbonate and TiO2
0.66 2.34

0.99 0.9
2.335
Refractive index of TiO thin film (n )
2

0.65
0.98 0.8
2.33
0.64 0.97 X: 1.58, Y: 2.3224 0.7
X: 120, Y: 0.63 Index: 1
2

Index: 1
Fill factor

0.96 2.325 0.6

0.63
0.95 2.32 0.5
0.62 0.94 0.4
2.315
0.93 0.3
0.61
2.31
0.92
0.2
0.6 0.91 2.305
115 120 125 1.565 1.57 1.575 1.58 1.585 1.59 1.595
Grating ridge height [nm] Refractive index of polycarbonate (n3)

Figure 2. FMM simulations show the relation between various design parameters at resonance wavelength (a) Variation between
TiO2 film thickness t and grating ridge height h, (b) Variation between incident angle θ and wavelength λ, (c) Variation between
grating ridge height h and fill factor f, (d) variation between refractive indices of polycarbonate (n3) and TiO2 (n2).

4. RESULTS AND DISCUSSION

The calculated reflectance spectra (TE-Mode reflectance) at room temperature and resonance wavelength (λr=855
nm) with full width half maximum FWHM of 10.7 nm is shown in figure 3a. The analysis of the spectral peak shift by
considering individual TEC, TOC and combined effects at 100 °C are shown in figure 3b. The analysis shows that under
thermal treatment, spectral changes appear which causes central resonance wavelength instable at all higher temperature
ranges. In figure 3b, spectral curve 1 shifts to longer wavelengths from its central position, this fact is attributed by
taking into account the contribution of thermal expansion coefficients TEC of polycarbonate and TiO2 films. The TEC
results to an increase in the periodicity, fill factor, ridge height of the structure profile. Thereby, due to expansion of
these parameters resonance wavelength shifts to slightly longer wavelengths and results to a spectral shift of 4 nm/75 °C

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above room temperature. Similarly, by considering the role of thermo-optic coefficients TOC of polycarbonate and TiO2
materials, a spectral shift is observed towards shorter wavelengths (curve 2). This effect is attributed to the fact that
refractive indices of both materials decrease with increase in temperature and causes a shift towards shorter wavelengths.
Thereby, due to negative TOC of these materials resonance wavelength corresponds to slightly shorter wavelengths and
results to a spectral shift of 3 nm/75 °C above room temperature. This effect is an inherent characteristic to all types of
dielectric bandpass filters being deposited by TiO2 coatings20. The choices of high TEC materials like polymers are more
effective and capable to partially counterbalance the shift towards shorter wavelengths. A combined result of the effects
revealed that the resonance wavelength stabilize partially close to its original stable position (at room temperature) and
shows a shift of ~1nm/75 °C which is 0.066 nm shift per 5 °C towards longer wavelengths. This observed shift is
relatively small in comparison with the FWHM of central spectral resonance. Most often these devices operate near room
temperature and a temperature variation of 25°C above room temperature results a shift of 0.333 nm which arise the
realization of partial athermalization of these devices.

Figure 3. Spectral reflectance of binary grating structure at resonance wavelength; (a) calculated central resonance wavelength at
room temperature (b) calculated central resonance wavelength at 100 °C due to, (1) TEC, (2) TOC and (3) combined effects.
Figure 4 shows the calculated spectral shift at a temperature of 100 °C with a temperature interval of 5 °C by
considering first the individual influences of TEC, TOC and their combined impact. The TEC effect in figure 4a shows
that spectral shift varies almost linearly with the temperature in all temperature ranges with a significant characteristic
slope of 0.0528. On the other hand TOC effect reveals a reverse spectral shift with rise in temperature; however, the shift
response is not exactly linear. One reason for this effect is the use of experimental values of index changes of TiO2 in our
computations which might be due to slight temperature fluctuations appeared during manual temperature control. In
addition, the refractive index changes of TiO2 shows linear relationships with density but predicted values of dn/dT are
not exactly linear with temperature which may be attributed due to some environmental effects, however, it can be
approximated as linear in our calculations with characteristic slope of 0.0388 as shown in figure 4b. The combined
behavior of both the factors TEC and TOC show a characteristic slope 0.0142 of spectral shifts with temperature which
is less than the either individual effects as shown in figure 4d. The calculations showed that effect of TOC (or
characteristic slope) is less than TEC which may be due to the fact of ALD coated TiO2 films with high refractive index.
The TiO2 films deposited by other techniques such as electron beam evaporation, ion-beam sputter deposition, RF diode
sputtering, ion or plasma plating, and activated reactive evaporation have refractive index values relatively less than
ALD coated films. The low refractive indices are due to porosity in the structure and low packing density of films. On
increasing temperature refractive index values for porous structures exhibit relatively more thermal-index-gradient than
high packing density TiO2 films by ALD process. It results relatively low value of negative index-gradient of ALD
coated films with temperature and subsequently low TOC with a small spectral shift towards shorter wavelength region.
Figure 5 shows the SEM picture of high index and amorphous TiO2 uniform cover layer on polycarbonate binary grating.
For exact athermalization, polymer optical materials of slightly low TEC might be employed with appropriate refractive
index and dn/dT values.

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 Figure 4. Effect of temperature on spectral shift (a) TEC factor only (b) TOC factor only (c) both TEC and TOC effects (d)
combines TEC and TOC effects showing partial athermalization phenomena.

Figure 5. SEM picture of high index amorphous TiO2 cover layer of thickness 61 nm by ALD on polycarbonate binary grating
substrate.

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 Thermal spectral measurements with temperature interval of 5 °C are performed by placing the sample on aluminum
hot plate. Measured data showed that efficiency of the grating would not effected significantly by increasing the
temperature as shown in Table 1. The resonance peak remains stable up to a temperature of 45 °C. The peak undergoes a
spectral shift of ~1nm from 826 to 827 nm in resonance wavelength when temperature rises from 45 to 50 °C while
remains stable during subsequent thermal measurements at higher temperatures up to 100 °C. Figure 6a shows the
overall experimental thermal spectral shift of ~1nm towards longer wavelength including both TEC and TOC effects on
rising temperature from 45 to 50 °C, indicating that TEC effect dominates over TOC contribution. The operation of these
devices up to 10’s of Celsius degrees above room temperature is successfully achieved without any spectral shift.
Calculated results shown in figure 3 are in agreement with experimentally measured results shown in figure 6. Both of
the results showed a spectral shift of ~1nm for a temperature change of 75 °C above room temperature towards longer
wavelengths. The calculated results showed that ~1nm shift is found at temperature of 100 °C whereas measured results
revealed same spectral change at 50 °C and further remains constant up to 100 °C without undergoing any change.
Thereby, perfect thermal shift stabilization could be achieved by selecting appropriate thermal expansion of polymeric
materials or by changing the thickness of the TiO2 cover layer.

Figure 6. Thermal spectral behavior of grating, (a) temperature rises from 45 to 50 °C; (b) Measured specular reflectance at room
temperature after subjecting to a temperature of 100 °C.
The grating was subjected to 100 °C (less than glass transition temperature of thermoplastics) during thermal
measurements, after then its spectral reflectance was re-measured at room temperature with the similar results that were
obtained before thermal treatment. This reveals that thermoplastic gratings do not undergo any permanent change of
which a decrease in its efficiency could result as shown in table1 and can be approximated to retrieve reversible spectral
behavior. It may be noticed that the grating exhibit a momentary swelling which may decrease the efficiency at higher
temperatures.

5. CONCLUSION

In this work high efficiency binary grating structures are designed and fabricated in optical thermoplastics
(polycarbonate) for TE-Mode operation around room temperature as partially athermalized devices. The athermalized
grating structures are the most economical and easy to fabricate for large scale production. The calculations include two
important factors, TEC and TOC. The FWHM at designed and measured resonance wavelengths are 10.7 and 13.5 nm
respectively. The design considerations come up by considering high TEC materials like optical polymer to
counterbalance and minimize the environmental effects on refractive index changes and high packing density TiO2
materials deposited by ALD. The TEC effect shifts the central resonance peak towards longer wavelengths ~4 nm
whereas TOC results a shift towards shorter wavelengths ~3 nm with characteristic slopes of 0.0528 and 0.038
respectively. The combined effect depends on both shifts show an average shift of ~1 nm towards longer wavelengths

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 Table 1. Measured specular reflectance and central resonance wavelength with temperature
Temperature (°C) Reflectance Resonance wavelength (nm)
25 0.970 826
30 0.970 826
35 0.948 826
40 0.933 826
45 0.915 826
50 0.904 827
55 0.888 827
60 0.862 827
65 0.828 827
70 0.791 827
75 0.749 827
80 0.730 827
85 0.703 827
90 0.726 827
95 0.649 827
100 0.469 827

with characteristic slope of 0.01421 with significant effect contributed by TEC. The experimental spectra are measured
up to 100 °C showing a spectral change of ~1nm towards longer wavelength, in complete agreement with theoretical
calculations. The experimental measurements show that shift occurs when temperature changes from 45 to 50 °C and
remains stable up to 100 °C. The efficiency is observed not more sensitive with temperature changes and retains at more
than 70 % up to 90 °C. The heated grating structures are re-measured at room temperature with the similar properties as
was measured before thermal treatment with complete reversible effects. This indicates that as long as the grating is
heated below glass transition temperature of polymers, it would not undergo any permanent change.

Acknowledgements
Financial support from the strategic funding of the University of Eastern Finland, Academy of Finland, Tekes,
Graduate School of Modern Optics and Photonics (Finland), and Higher Education Commission HEC (Pakistan) are
greatly appreciated.

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