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1.—Centre for Applied Research in Electronics, Indian Institute of Technology Delhi, Hauz-Khas,
New Delhi 110016, India. 2.—e-mail: schandra@care.iitd.ernet.in
1979
1980 Bhatt and Chandra
sequential deposition, low cost, and a simpler microcantilever beams were fabricated using bulk,
deposition system. Furthermore, the lower deposi- surface, and surface-bulk micromachining tech-
tion temperature of RF sputtering is beneficial niques. For microelectronic and MEMS application,
when fabricating devices that monolithically inte- the use of RF-sputtered silicon nitride film as a
grate silicon nitride with temperature-sensitive mask against oxidation in the LOCOS process has
materials such as mercury cadmium telluride and been explored.
organic or biomaterials. Many researchers have
reported the deposition of silicon nitride by the FILM DEPOSITION
RF-sputtering process.16–20 Silicon nitride depos- AND CHARACTERIZATION
ited by LPCVD and PECVD is widely used as a
Film Deposition
structural material in the fabrication of different
MEMS devices, such as static membranes, tunable The silicon nitride films were deposited in an RF
inductors, and tunable MEMS Fabry-Pérot optical (13.56 MHz) diode sputtering unit (Alcatel, QM-311).
filters.6–9,21,22 However, sputtered silicon nitride A diffusion-pump-based vacuum system with
has not yet been explored as a structural layer in liquid-nitrogen trap was used. A high-purity silicon
MEMS. This is the main motivation for the present nitride (Si3N4) target with 75 mm diameter and
work. 5 mm thickness was fixed to the water-cooled target
In this paper, we report low-temperature holder with conducting epoxy. The sputtering was
(<260°C) RF-sputtering deposition of silicon nitride done in argon ambient in the ‘‘sputter-up’’ configu-
film for structural layers in MEMS. The influence of ration. The sputtering pressure was in the range of
sputtering parameters such as RF power, sputter- 5 mTorr to 20 mTorr and the RF power was varied
ing pressure on deposition rate, etch rate, surface from 100 W to 300 W. The distance between the
roughness, and residual stress in the film has been target and the substrate was kept constant at
investigated. Silicon nitride films were deposited on 45 mm. Both-side optically polished transparent
single/double-side polished silicon and transparent fused-quartz discs of 1 inch diameter and single- or
fused-quartz substrates by RF sputtering of a silicon double-side polished (100)-oriented 2-inch-diameter
nitride (Si3N4) target in an argon ambient. The silicon wafers were used as the substrates. Prior to
optical and microstructural properties of the films deposition, the substrates were cleaned in hot (90°C
were evaluated by ultraviolet–visible (UV–Vis) to 100°C) H2SO4:H2O2 (1:1) solution for 15 min fol-
spectroscopy, Fourier-transform infrared (FTIR) lowed by deionized (DI) water rinse. After this step,
spectroscopy, scanning electronic microscopy the silicon substrates were immersed in 5% HF for
(SEM), and atomic force microscopy (AFM). Stress 30 s to remove the native oxide formed in the hot
control in the deposited films, especially when these H2SO4:H2O2 solution. The wafers were rinsed in
are employed as a structural layer in MEMS, is very running DI water and spin-dried. After loading the
important because too much intrinsic tensile stress samples, the chamber was evacuated to a base
causes the bridge/membrane to fracture, while pressure of 2 9 106 Torr and then throttled. Before
compressive stress results in upward or downward starting the deposition, the target was sputter-
buckling. The deposition parameters for obtaining cleaned for 10 min. All the depositions were carried
films with minimum residual stress, lower surface out without any external substrate heating. The
roughness, and lower etch rate were optimized. To deposition parameters for the preparation of various
demonstration RF-sputtered silicon nitride films samples on both types of substrates are summarized
as a structural layer in MEMS, silicon nitride in Table I.
Table I. Deposition Rate, Refractive Index, and Etch Rates of Films Prepared Under Different Process
Parameters
Etch Rate
Sputtering Deposition Rate Refractive Etch Rate in 40 wt.%
Sample RF Pressure at the Center Index in BHF Aqueous KOH
Name Power (W) (mTorr) of the Wafer (Å/min) (n) (Å/min) at 70°C (Å/min)
Deposition Rate
The deposition rate is a very important parameter
for controlling the required film thickness at a given
target-to-substrate spacing, sputtering pressure,
and RF power, especially for precise multilayer
coating. The deposition rate was obtained by mea-
suring the film thickness using a thin-film analyzer
(Filmetrics F20, USA) and deposition time. The
same system can also used for measuring the
refractive index n(k) and extinction coefficient k(k)
of the films.
Figure 1 shows the deposition rate of films as a
function of sputtering power at 5 mTorr, 10 mTorr,
and 20 mTorr sputtering pressure. The maximum
deposition rate is obtained at the centre of the
2-inch silicon wafer. Near the periphery of the
wafer, the deposition rate falls by around 5% for all
samples. The deposition rate exhibits strong Fig. 2. Change in substrate temperature with sputtering time for
dependence on the RF power and increases with different RF powers at 10 mTorr pressure.
increasing sputtering power, which is consistent
with published results.
10 mTorr, 100 W
Si-N bonds
10 mTorr, 200 W
Transmittance (arb. unit)
10 mTorr, 300 W
Si-OH bonds
Si-N bond shifted
towards Si-O bond
power exhibit a strong absorption band centered determined from the change in the radius of
around 840 cm1 to 860 cm1, which corresponds to curvature of the wafer, before and after film depo-
the stretching vibration mode of the Si-N bond.13 sition, using a 500TC temperature-controlled film
In this configuration, silicon atoms are nearly tetra- stress measurement system (FSM Frontier Semi-
hedrally surrounded by four nitrogen atoms. The conductor). The substrate curvature method relies
large value of the full-width at half-maximum of on the Stoney formula relating the average stress of
this band is consistent with previously reported the film to the substrate curvature under the
work,13 and is attributed to the amorphous nature assumption that the film is much thinner than the
of the silicon nitride films. The additional small underlying substrate.24 The stress in a thin film of
absorption band observed at 480 cm1 corre- thickness df can be expressed as
sponds to Si–N breathing mode.13 We also observed
that samples deposited at 100 W RF power showed Es d2s 1 1
a larger shift toward higher frequency. rf ¼ ; (1)
6ð1 ms Þdf Rf R0
Optical Transmittance where Es, ms, and ds are the Young’s modulus,
Poisson ratio, and thickness of the substrate,
The optical transmission and reflection spectra
respectively, and R0 and Rf are the radii of substrate
were obtained for the films deposited on quartz
curvature before and after film deposition.
substrates in the wavelength range of 200 nm to
Figure 5 shows the dependence of the stress on
2000 nm using a Perkin-Elmer Lamda 900 UV–Vis
the sputtering pressure for 1-lm-thick silicon
spectrometer. For these measurements, a 500-Å-
nitride film deposited at 100 W to 300 W RF power.
thick silicon nitride film was deposited on 1-inch-
As seen from Fig. 5, the stress in the films is com-
diameter quartz substrates.
pressive in the entire pressure range investigated,
Transmittance spectra for films prepared under
and decreases from 1360 MPa to 390 MPa as the
different deposition conditions (Table I) were
sputtering pressure is changed from 5 mTorr to
obtained in the 200 nm to 2000 nm wavelength
20 mTorr for the film deposited at 300 W RF power.
range. Figure 4 shows the transmittance spectra of
At lower sputtering pressures, the inelastic collision
the samples deposited at 10 mTorr pressure with
probability between plasma particles decreases,
varying RF power (100 W, 200 W, and 300 W). The
enhancing the peening effects of the energetic
samples exhibit absorption edges at different
plasma particles.25,26 Therefore, the intrinsic stress
wavelengths in the ultraviolet region, which indi-
increases with decreasing pressure. In the case of
cates varying absorption characteristics with depo-
silicon nitride, deposition at higher pressure seems
sition conditions. These spectra show that the
to be favorable for obtaining low stress.
silicon nitride films exhibit good optical transpar-
Figure 6 show the effect of film thickness on the
ency in the visible and near-infrared regions.
stress in the silicon nitride films. All the films were
deposited at 10 mTorr pressure and 300 W RF
Stress Measurement
power. From Fig. 6 it is clear that the stress in the
The residual stress in the films deposited on silicon nitride film is compressive in nature and
2-inch single-sided polished (100) silicon wafers was decreases as the film thickness is increased from
Surface Roughness
The average surface roughness of the deposited
films is a critical parameter when these are
employed as an intermediate layer for wafer bond-
ing processes and for optical surface in MOEMS
devices and micromirror. An AFM was used for
measuring surface roughness. The AFM measure-
ments (surface roughness) of silicon nitride films
deposited at 100 W to 300 W RF power and at dif-
ferent sputtering pressures were carried out using a
Digital Instruments Nanoscope IIIA apparatus. The
films were deposited on high-quality n-type (100)-Si
pieces of size 10 mm 9 10 mm. The film thickness
was kept constant at 5000 Å except where surface
roughness was considered as a function of film
thickness. All the images have the same scanning
area of 4 lm 9 4 lm.
Fig. 6. Dependence of residual stress in the silicon nitride film on Figure 8a–c shows three-dimensional AFM ima-
film thickness. ges of 5000-Å-thick silicon nitride films deposited on
silicon at 5 mTorr, 10 mTorr, and 20 mTorr pres-
sure, respectively, and at 300 W RF power. It is
clear from the images that the surface roughness
increased significantly with higher sputtering
pressure. This sputtering pressure dependence is
shown in Fig. 9, which shows that the roughness
was significantly low at lower sputtering pressure.
Atomic peening, caused by reflected high-energy
neutral species and the increased energy of sputter
gas atoms, might be the possible reason for the
smoother films at low pressure, since this phenom-
enon densifies the deposited films at low pres-
sure.25,26 The atomic peening effect decreases as the
pressure is increased. This pressure dependence can
also be explained by the gas scattering effect: the
number of scattering events in the path from the
target to the substrate increases with increasing
deposition pressure. Scattering reduces the energy
of sputtered particles and increases their angular
distribution. Less energy of sputtered particles
leads to reduced mobility on surface, while the
Fig. 7. Residual stress versus annealing time for silicon nitride films increased angular distribution enhances shadow-
deposited at 300 W RF power and 10 mTorr pressure for different ing. The contribution of these two factors results in
thicknesses.
a rougher surface at a higher sputtering pressure.
Figure 9 also shows the effect of sputtering power
on the surface roughness. From Fig. 9, it is observed
0.5 lm to 2 lm. Deposition time is higher to obtain that the surface roughness of the film decreases
thicker films, which provides more time for stress when the sputtering power increases. The surface
relaxation during deposition and results in lowering mobility or diffusion of the sputtered atoms affects
of the stress in the films. Alternatively, with the growth mechanism of the film. This mobility can
increase in the thickness of the silicon nitride film, be enhanced by inputting more energy to the system
the electrical insulation over the substrate (silicon) such as increasing the deposition temperature or
increases, which may alter/reduce the energy of the supplying impact energy through ion bombardment.
incoming species (probably positive ions) due to the At high RF power (300 W), the kinetic energy of
bias over the substrate. sputtered ion/atoms increases and also the sub-
Figure 7 shows the effect of annealing time on the strate temperature increases due to self-heating
stress in the silicon nitride film of different thick- (Fig. 2). These two factors enhanced surface diffu-
nesses deposited at 10 mTorr pressure and 300 W sion and smooth the growth front, resulting in a
RF power. From Fig. 7 it is observed that the stress lower surface roughness. On the other hand, at low
is released through the annealing process and RF power, ions have low energy and the substrate
decreases initially with annealing time. temperature is also low due to lower self-heating.
1984 Bhatt and Chandra
(a) (b)
1 1
2 2
x 1.00 µm/div x 1.00 µm/div
3 3
µm z 50.00 nm/div z 50.00 nm/div
µm
(c)
1
2
3 x 1.00 µm/div
µm z 50.00 nm/div
Fig. 8. Atomic force micrographs of silicon nitride films deposited at 300 W RF power at (a) 5 mTorr, (b) 10 mTorr, and (c) 20 mTorr pressures.
The scanned area is 4 lm 9 4 lm and the film thickness is 0.5 lm for all the samples.
Fig. 9. Variation of surface roughness (Ra) as a function of Fig. 10. Surface roughness (Ra) versus thickness of silicon nitride
sputtering pressure at different RF powers. films deposited at 300 W RF power and 10 mTorr sputtering pressure.
Ions are therefore more likely to stay at the site of roughness is observed to decrease as the film
arrival, thus creating a rougher surface. Figure 10 thickness increases from 0.5 lm to 2 lm. The
presents the effect of film thickness on the surface deposition time for preparing thicker films is
roughness (Ra) deposited at 300 W RF power and greater, which allows the atoms to rearrange into
10 mTorr sputtering pressure. The average surface low-energy states by surface diffusion. This may be
Silicon Nitride Films Deposited by RF Sputtering for Microstructure Fabrication in MEMS 1985
(100)-Si
(b) lithography (using mask 1) and etching of the Figure 16 shows SEM photographs of completely
oxide in BHF followed by anisotropic etching of Si in planar microcantilever beams.
KOH to create 3-lm-deep cavities of different sizes,
(c) global etching of oxide, (d) deposition of PSG by
RF-SPUTTERED SILICON NITRIDE
RF sputtering (thickness is more than cavity depth),
AS A MASK IN OXIDATION
(e) pattering of PSG film using mask 2, (f) planari-
zation by CMP using Mastermet colloidal silica An RF-sputtered silicon nitride film was explored
polishing suspension (Buehler Co.), (g) deposition of as a mask in thermal oxidation processing.
1.5-lm silicon nitride (as a structural material) by Figure 17 shows a schematic view of the process
RF sputtering at 300 W and 10 mTorr pressure, (h) sequence used in LOCOS. The process was per-
photolithography and etching of silicon nitride film formed on a silicon substrate having 2000 Å silicon
by RIE using SF6 gas (mask 3), and (i) removal of nitride deposited over 500 Å SiO2 (pad oxide, ther-
RF sputtered PSG in BHF. Following the PSG etch, mally grown). Silicon nitride film was deposited by
the samples were rinsed in two successive DI water RF sputtering at 300 W power and 10 mTorr pres-
baths, each lasting for 5 min, followed by a 10-min sure. After silicon nitride deposition, the lithogra-
dip in acetone. The final rinsing was done for 10 min phy was performed to open windows. Silicon nitride
in a surface-tension-weakening solution (methanol) was etched in SF6 plasma (RIE mode) and the
and the wafers were dried under an IR lamp. pad oxide in BHF. Figure 18 shows an optical
1988 Bhatt and Chandra
Fig. 19. SEM micrograph showing typical bird’s beak in the LOCOS
process.
(d) Removal of nitride
(100)-Si SiO2
It was observed that the combined thickness of
Deposited silicon nitride silicon nitride-pad-SiO2 remained unchanged after
Fig. 17. Schematic process sequence of the LOCOS process. the thermal oxidation. It was further confirmed that
the pad oxide thickness was also not affected after
removing the silicon nitride globally. Figure 19
photograph of silicon nitride lines after patterning shows an SEM photograph of the bird’s beak after
and etching process. Total thickness of silicon the LOCOS process. These observations demon-
nitride/pad oxide was measured by alpha step before strate that an RF-sputtered silicon nitride film
thermal oxidation. Wet oxidation at 1000°C was can be advantageously used for LOCOS isolation
then carried out for 1 h. After oxidation, silicon technology.
nitride was globally etched out in orthophosphoric
acid. The oxide thickness was measured on areas CONCLUSIONS
that were protected by silicon nitride during the Silicon nitride films deposited at low tempera-
oxidation process. SEM was used to observe the tures (<260°C) by RF sputtering have been inves-
bird’s beak, which is typical in the LOCOS tigated for application in MEMS. The effect of
process.29 deposition parameters such as RF power and
Silicon Nitride Films Deposited by RF Sputtering for Microstructure Fabrication in MEMS 1989
sputtering pressure on the chemical bonds, optical 6. K.J. Winchester and J.M. Dell, J. Micromech. Microeng. 11,
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7. L. Wang, Z. Cui, J.S. Hong, E.P. McErlean, R.B. Greed, and
rates were studied. It was observed that these D.C. Voyce, Microelectron. Eng. 83, 1418 (2006). doi:10.1016/
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