Ping Hou

Nortel Networks Co.

Richard Sun
Angstrom Sun Technologies Inc.

Presented at MRS Fall Meeting 2002 in Boston

Introduction
Titanium oxide (TiO2) thin film has been widely used as optical coatings due
to its high index of refraction. It is well known that structures and properties of
TiO2 films are highly dependent on the processing techniques. E-beam
evaporation has long been recognized as a practical way of depositing optical
thin films. However, preparing a homogenous TiO2 film with this technique is
still a challenge. One of the difficulties of getting a structurally uniform TiO2 film
lies in the fact of its low phase transformation temperature. It is vital to find a
fast and non-destructive way to monitor and evaluate the film optical quality. It
is also important to tail the film stress at will to satisfy mechanical requirements
for MEMs devices, such as vertical cavity surface emission laser (VCSEL). To
this end, the stress and structural homogeneity of e-beam evaporated TiO2
films will be examined and discussed in this research.
Deposition Chamber

Crystal 3
Sample Holder 2
1 3

Heater
Ion Gun

SiO2 TiO2
 Deposition Process

Table 1. Experiment Conditions for Structural Study

Deposition Rate (/s) 2.0

Chamber Pressure (Torr) 2.510-4
Anode Voltage (V) 130
Anode Current (A) 1.0

Table 2 Experimental Conditions for Stress Study

Deposition Rate (/s) 2.0 2.5 3.0

Chamber Pressure (Torr) 2.010-4 2.510-4 3.010-4
Anode Voltage (V) 100 130 160
Anode Current (A) 1.0 2.5 3.5
 Model and Its Analyses
RP
= S = Tan e j = f (ni , k i , d i )
R
Measured Data Physical Model
Estimated sample structure
Tan - Film Stack and structure
- Material n, k, dispersion
Cos - Composition Fraction of Mixture

Measurement No
=
Calculation ?

Yes

Ti , ni , ki
Refractive Index Profile

Substrate
Analysis Model

Lower
Part
TiO2 Film

Middle
Part

Upper Part
 Spectra FittingsThree Sub-Layer Model

0.7 1.2
Fitted Tan(Psi)
Measured Tan(Psi)
0.6 1

0.5 0.8

0.4
Tan (Psi)

0.6

Cos (Del)
0.3 0.4

0.2 0.2

0.1 0
Fitted Cos(del)
Measured Cos(del)
0 -0.2
0.62 1.12 1.62 2.12 0.62 1.12 1.62 2.12
eV eV

With the three Sub-layer model, the whole spectra can be successfully
fitted for a as-deposited TiO2 film, indicating a heterogeneous structure.
Graded Optical Constants of TiO2 Film
2.6

Upper Part
2.5
Middle Part
Lower Part
2.4

2.3
Refractive Index (n)

2.2

2.1

1.9

1.8

1.7
0.5 0.7 0.9 1.1 1.3 1.5 1.7 1.9
Wavelength, um

Ellipsometry analysis shows the gradient refractive index from the film/substrate
interface to top of the film. The typical values at 1550 nm wavelength are 1.721
(upper part), 2.2363 (middle part), and 2.2825 (lower part), respectively.
 Microscope Observation

(a) (b)

(a) SEM photo showing three sub-layers of an as-deposited TiO2 film (left); (b) TEM photo for
alternating SiO2/TiO2 multiple layers shows the same structure for TiO2 single layer (right)
Chamber Temperature Variance

240

Chamber Temperature (C) 230

220
210
200
190
180
170
160
150
0 5 10 15 20 25 30 35 40

Deposition Tim e (m in)

It was the temperature variance that caused the

structural discrepancy of as-deposited TiO2 film.
 Co-deposited TiO2-SiO2 Film

Ellipsometry analysis shows an excellent fitting for a co-evaporated TiO2-SiO2

film with only one layer model simulation, indicating a homogeneous structure.
Surface Micrographs

(a) (b)

TiO2 Film Co-evaporated TiO2-SiO2 Film

SEM micrographs show (a) an as-deposited TiO2 film (left) and (b) a TiO2-SiO2
co-evaporated film (right). AFM analysis shows that the surface roughness of
pure TiO2 film and co-evaporated film are 19.6 and 9.3 nm, respectively.
 TiO2 Film Stress Dependency
300 285
Anode Current: 1.0A
250 280

275
200
Stress (MPa)

Stress (MPa)
270
150
265
100
260
50 255

0 250
1 2 3 2 2.5 3
-4
Deposition Rate (/s) Cham ber Pressure (10 Torr)

400
300
300
290
200
Stress (MPa)

Stress (MPa)
280 100

270 0
1.0 2.0 3.5
260 -100

-200
250
-300
240 -400
100 130 160 Anode Current (A)
Anode Voltage (V )

Any process that can increase the film packing density will result in decreasing tensile
stress, or increasing compressive stress. Therefore, low deposition rate, high-energy
or intensive ion bombardment will produce more compressive stress for as-deposited
TiO2 films.
 Summary
TiO2 film stress can be tuned through properly adjusting the
deposition parameters, especially anode current of the ion gun.

Spectroscopic ellipsometry has been successfully used as a

nondestructive technique to characterize the structural discrepancy
of TiO2 films.

Three sub-layer model can be used to describe the heterogeneity

of as-deposited TiO2 films, which is caused mainly by the chamber
temperature changes during the deposition.

With TiO2-SiO2 co-deposition, a homogeneous film can be

produced. At the same time, refractive index can be further tuned
through controlling the ratio of TiO2 to SiO2 fraction in the film.

ACKNOWLEDGEMENT
The authors thank colleagues for SEM/TEM analyses and any other assistance