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Journal of the Korean Physical Society, Vol. 42, February 2003, pp.

S947S951

Optical Characterization of Silica Based Waveguide Prepared by Plasma


Enhanced Chemical Vapor Deposition
S. M. Cho, Y. T. Kim and D. H. Yoon
Department of Advanced Materials Engineering, Sungkyunkwan University, Suwon 440-746

J. M. Kim, H. D. Yoon and Y. M. Im


Optical Telecommunication Research Center, Korea Electronics Technology Institute, Pyungtaek 451-865

G. E. Jang
Department of Materials Science & Materials Engineering, Chungbuk University, Cheongju 361-763
Silicon dioxide (SiO2 ) and silicon oxynitride (SiON) thick films used for cladding and core layer
of silica based waveguides were fabricated by plasma enhanced chemical vapor deposition (PECVD)
method, at a low temperature (320 C) and from (SiH4 +N2 O+N2 ) gas mixtures. The effects of
deposition parameters on properties of SiO2 and SiON thick films were investigated by variations
of SiH4 , N2 , N2 O flow ratio and RF power. The obtained SiO2 films had a high thickness and
refractive index of 1.4600.001 with the annealing process. FTIR and XPS revealed that deposited
films were nearly stoichiometric composition with no presence of hydrogen content. SiON films had
a 0.75 % higher refractive index than the cladding layer and a high thickness(> 5 m).
PACS numbers: 81.15.Gh, 78.66.-w
Keywords: PECVD, Optical waveguide, Silicon dioxide, Silicon oxynitirde

I. INTRODUCTION
Various kinks of optical components are required
for implementation optical communication systems with
higher transmission efficiency.
These components
include optical beam splitters/combines for branching/combining optical signals, optical switches for changing optical paths for flexible network utilization, and
wavelength-division multi/demultiplexers for introducing multiple optical channels into a single optical fiber
[1]. Silica waveguide systems with glass composition are
similar to that of optical fibers. Silica waveguides can be
formed on crystal silicon substrates by a combination of
glass film deposited and etching. Their simple and clear
core structures, low propagation loss are almost perfect
field matching to optical fibers. The formation technique
of the SiO2 based waveguide is required for the fabrication of a planar waveguide device which is necessary for
broad-band optical communication technique [2,3].
Flame hydrolysis deposition (FHD) [4], chemical vapor deposition (CVD) [5] and plasma enhanced chemical vapor deposition (PECVD) [6,7] are usually used for
fabrication of silica waveguides. The FHD process can
fabricate a thick SiO2 layer in a short time and has the
advantage of low optical loss and easier coupling with
optical fiber. But it is difficult to control the dopant and
flame. Moreover, the FHD process is required the consolidation process at a higher temperature about 1300

C. Chemical vapor deposition (CVD) and its variants,


such as modified chemical vapor deposition (MCVD) and
plasma enhanced chemical vapor deposition, can all produce thin layers of deposited silica or doped silica by
using admixtures of either vapor or gases. MCVD relies
on thermal heating for the creation and deposition of the
glass soot, whereas PECVD and its variants rely on ionic
catalysts. One advantage of PECVD, over both FHD
and other CVD processes, is that it is a low-temperature
process, compatible with temperatures occurring in microelectronics processing.
In this study we discuss the fabrication of silica
waveguides on silicon substrate, describing the lowtemperature PECVD process and the relationship of between optical characterizations and processing parameters.

II. EXPERIMENT
Silicon dioxide (SiO2 ) and silicon oxynitride (SiON)
films were deposited by PECVD having a radio frequency
plasma using a standard 13.56 MHz source in a popular parallel plate electrode. P-type Si (100) wafers were
cleaned by the RCA process consisting of immersion in
a piranha (H2 SO4 :H2 O2 =4:1) solution for 10 min at 80

C, a deionized water (DI) rinse and immersion in a 1

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Journal of the Korean Physical Society, Vol. 42, February 2003

Fig. 1. Refractive index and deposition rate of SiO2 films


as a function of N2 O/SiH4 flow raito.

% HF for 40 s. After a final DI rinse and a nitrogen


blow dry, the substrates were loaded to chamber and
cleaned by N2 plasma sputtering. For the growth SiO2
films on the substrate, high purity silane (SiH4 , 90 %
dilution H2 ), nitrogen (99.99 % N2 ) and nitrous oxide
(99.999 % N2 O) were used. Gas input was controlled by
the Mass Flow Controller (MFC) and low evacuation was
done through a double stage rotary pump and booster
pump. Pre-deposition evacuation was pumped at the
105 torr range by using a diffusion pump.
The effects of the deposition parameters on properties
of SiO2 and SiON thick films were investigated by variations of the SiH4 , N2 O, N2 flow ratio and RF power. After the deposition process, the samples were annealed in
a furnace at 1150 C for 2h. Lithography processes were
then used to deposit a predesigned mask on the top of
the core layer. Chrome was used for the mask materials.
The silica waveguide layer was etched by Inductive Coupled Plasma (ICP) etching system. The thickness and
the refractive index measurements were measured by a
prism coupler. X-ray photoelectron spectroscopy (XPS)
and fourier transform infrared spectroscopy (FTIR) were
used to determine the chemical states. The cross-section
of films was observed by a scanning electron microscopy
(SEM).

III. RESULTS AND DISCUSSION


1. Silicon dioxide films

In a typical fabrication process, a uniform buffer layer


of pure silica is deposited on the surface of the wafer
to a depth of the order of 10 or more. The effects of
the reactant gas flow ratio on the growth characteristics
and optical properties were investigated by changing the
N2 O/SiH4 flow ratio and RF power. Fig. 1 shows the
variation of the growth rate and refractive index with

Fig. 2. Refractive index and deposition rate of SiO2 films


as a function of RF power.v

the N2 O/SiH4 flow ratio. The pressure, RF power and


temperature were 0.9 torr, 120W and 320 , respectively.
It is observed that the deposition rate was decreased
by the depletion of silane as the N2 O/SiH4 flow ratio
increased. Refractive index decreased approaching the
thermally grown SiO2 (1.46) as the flow ratio increased
from 3 to 22. After annealing process, Si-O-Si bonds
were increased and SiO2 films having a stoichiometric
composition were formed [8].
Fig.
2 shows the variation of the growth rate
and refractive index with RF power. The pressure,
N2 O/SiH4 flow ratio and temperature were 0.9 torr, 8
and 320 , respectively. RF power varied from 60 to
180W. Deposition rate was increased from 4.7 /h to 6.9
/h resulting in a higher fractional ionization and a denser
plasma as the RF power increased. Refractive index had
an index range of 1.460 0.001 at the RF power above
120 W. After the annealing process, the deposition rate
and the refractive index were decreased. It can be explained by a desorption of Si-N and Si-H bondings adsorbed in the surfaces of samples as a function of annealing.
The structural and bonding properties of SiO2 thick
films as an annealing process are revealed in Fig. 3. Hydrogen content induces bad optical characteristics into
the silica waveguide [911]. O-H, Si-OH and Si-H bondings can be detected by fourier transform infrared spectroscopy (FTIR). It is observed that Si-H, Si-O-H bondings are detected at 2300 cm1 , 960 cm 1 respectively
for non-annealing. After the annealing process, Si-H,
Si-O-H bondings are not detected and Si-O-Si stretching and bending mode are detected at 1068 cm1 , 845
cm1 . It is known that the stretching frequency of the
Si-O bonds is related to the films stoichiometry.
Films stoichiometry is also identified by the XPS spectrum using the O 1s and Si 2p binding energy. In case of
stoichiometry SiO2 , the silicon atom surrounded by four
oxygen atoms has a characteristic binding energy (103.3
eV). Because carbon appeared at the oxide surface due
to the contamination from the atmosphere, carbon was

Optical Characterization of Silica Based S. M. Cho et al.

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Table 1. Deposition Condition of SiO2 films.


Sample
SO-1
SO-2
SO-3
SO-4
SO-5
SO-6
SO-7
SO-8
SO-9
SO-10

Temp. ( )

Deposition pressure (torr)

RF power (W)

320

0.9

0.9

320

Variable constant

150

N2 O/SiH4 flow ratio


3
6
8
10
14
22

60
90
120
180

RF power

used for reference (284.5 eV). Fig. 4 shows the chemical


bonding state of silicon and oxygen. The binding energy of Si 2p and O 1s was 103 and 532 eV, respectively.
It is confirmed that deposited films has a stoichiometric

N2 O/SiH4 flow ratio

composition.
As the condition of N2 O/SiH4 flow ratio and RF power
are 8 and 120 W, respectively high quality SiO2 thick
film having an 18 m thickness was deposited and its
cross-section is revealed in Fig. 5.

2. Silicon oxynitride films

Fig. 3. IR spectrum of SiO2 films as annealing process (a)


before annealing and (b) after annealing.

Fig. 4. XPS Si 2p and O 1s line shape of SiO2 films.

The core index must be slightly higher than the


cladding index in order to provide light guidance, and
also to be compatible with the core-cladding index difference of standard telecommunications single mode fibers
which are spliced to the planar devices. The higher index
of the core layer can be achieved by doping with nitrogen. The effects of the reactant gas flow ratio on the
growth characteristics and optical properties were investigated by changing the (N2 O + N2 )/SiH4 flow ratio and
RF power. Fig. 6 shows the variations of the growth rate
and the refractive index with the (N2 O + N2 )/SiH4 flow
ratio. The pressure, RF power and temperature were
0.9 torr, 150 W and 320 C, respectively. The deposition rate was decreased from 8.7 m/h to 2.1 m/h as

Fig. 5. SEM photograph of SiO2 thick film.

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Journal of the Korean Physical Society, Vol. 42, February 2003

Table 2. Deposition Condition of SiON films.


Sample
ON-1
ON-2
ON-3
ON-4
ON-5
ON-6
ON-7
ON-8
ON-9

Temp. ( C)

Deposition pressure (torr)

RF power (W)

320

0.9

0.9

320

Variable constant
(N2 O+N2 )/ SiH4 flow ratio

150

(N2 O+N2 )/SiH4 flow ratio


3
4
6
10
20

60
90
120
180

RF power

the (N2 O + N2 )/SiH4 flow ratio increased. For a small


(N2 O + N2 )/SiH4 flow ratio, Si-N and N-H bonds which
formed by preference reaction between silane radical and
oxygen radical are incorporated into the films, so refractive index has a high value. As the (N2 O + N2 )/SiH4
flow ratio increased, the refractive index decreased approaching the 1.4710 that had a 0.75 % difference with
the cladding index.
Fig. 7 shows the variations of the growth rate and
the refractive index with the RF power. The pressure,
(N2 O+N2 )/SiH4 flow ratio and temperature were 0.9
torr, 6 and 320 C, respectively. As the RF power increased, the deposition rate was increased from 4.4 m/h
to 6.7 m/h by the high dissociation. For lower RF
power, silane decomposes more easily than nitrous oxide [12], so Si-H and N-H bonds are preformed and the
refractive index is increased. As RF power increased,
the refractive index was decreased by higher nitrous oxide dissociation. As the condition of (N2 O+N2 )/SiH4
flow ratio and RF power are 6 and 150W, SiON thick
film having an 8 m thickness was deposited and its refractive index was 1.4705.
Having a above results, we fabricated the cladding and
core layer which were 15 m and 8 m in thickness, re-

Fig. 7. Refractive index and deposition rate of SiON films


as a function of RF power.

spectively. The silica waveguide layer was etched by ICP


etching system. Fig. 8 shows the SEM photograph of the
SiON thick film and etched core ridge of a single-mode
waveguide. The waveguide in Fig. 8 has a relative refractive index difference between the core and cladding of
0.75 %.

IV. CONCLUSIONS

Fig. 6. Refractive index and deposition rate of SiON films


as a function of (N2 O + N2 )/SiH4 flow raito.

In this study, we have deposited SiO2 and SiON thick


films by PECVD at low temperature and have shown the
relationship between the optical properties and the process parameters. The obtained SiO2 films had a high
thickness and refractive index of 1.460 0.001 with
the annealing process. FTIR and XPS revealed that
deposited films were nearly stoichiometric composition
with no presence of hydrogen content. SiON films using
a core layer had a 0.75 % higher refractive index than
the cladding layer and a high thickness(> 5 m). We
could note that film thickness and refractive index were
controlled by the flow ratio of the reactant gas, the RF
power and the annealing process.

Optical Characterization of Silica Based S. M. Cho et al.

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Fig. 8. (a) SEM photograph of SiON thick film. (b) SEM


photograph of etched core ridge of a single-mode waveguide
by ICP etching system.

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