Reactivesputter deposition and structure of RuO2 films on sapphire and strontium

titanate
Q. Wang, Wayne L. Gladfelter, D. Fennell Evans, Yue Fan, and Alfonso Franciosi
Citation: Journal of Vacuum Science & Technology A 14, 747 (1996); doi: 10.1116/1.580382
View online: http://dx.doi.org/10.1116/1.580382
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Reactive-sputter deposition and structure of RuO2 films on sapphire

and strontium titanate
Q. Wang, Wayne L. Gladfelter, D. Fennell Evans, Yue Fan, and Alfonso Franciosi
Department of Chemistry and Department of Chemical Engineering and Materials Science, University of
Minnesota, Minneapolis, Minnesota 55455

~Received 5 October 1995; accepted 22 January 1996!

Metallic films of RuO2 were deposited by reactive-sputtering deposition on single crystal substrates
of Al2O3 ~0001! and SrTiO3 ~100! at room temperature and 450 C. Measurement of the
characteristic hysteresis loop revealed that the targets transition from a metal to a metal oxide
surface occurred at a very high O2/Ar ratio ~88%! under our experimental conditions. The
hysteretical behavior of the transition was evaluated experimentally and was modeled.
Resonance-enhanced Rutherford backscattering spectrometry established that the films deposited at
450 C had an oxygen to ruthenium ratio of 1.97, while a slightly higher value of 2.08 was observed
for the films grown at room temperature. The latter films were amorphous, whereas those grown at
450 C exhibited a highly oriented polycrystalline microstructure. On SrTiO3 ~100!, the RuO2 ~100!
plane is parallel to the substrate surface, but no in-plane orientation was found. The same face, RuO2
~100!, was also parallel to the surface of Al2O3 ~0001!, and the @001# direction of individual grains
of RuO2 aligned with the three ^ 1 010& directions of the substrate to produce a threefold mosaic
microstructure. 1996 American Vacuum Society.

I. INTRODUCTION
Ruthenium dioxide exhibits metallic conductivity ~r535
mV cm! and very high thermal and chemical stability; these
properties make RuO2 valuable for a variety of applications.13 Reactively sputtered RuO2 films have been demonstrated to be an excellent diffusion barrier between Al and Si
in very large scale integrated ~VLSI! circuits,3,4 and RuO2
has been used as a diffusion barrier and stable base electrode
for ferroelectric2,5 and high-T c superconducting metal oxide6
thin films. The rutile structure of RuO2 allows anisotropic
diffusion of impurities where the mass transport along the c
axis is faster than in the directions perpendicular to it.3 This
anisotropy makes the microstructure of RuO2 films a crucial
factor for its applications.
Although RuO2 film has been grown by several different
techniques,3,79 no consistent conclusion has been reached
regarding the factors controlling stoichiometry and microstructure of reactively sputtered RuO2 films. For instance,
previous studies of RuO2 grown by reactive sputtering have
reported O:Ru ratios varying from 0.5 to 2.4.10 In this article
we will first describe the reactive sputtering kinetics of RuO2
film growth. The hysteretical behavior was measured experimentally and modeled using the procedures outlined by Berg
and co-workers.11,12 The composition and microstructure of
RuO2 films grown on Al2O3 ~0001! and SrTiO3 ~100! single
crystal substrates will be discussed.
II. EXPERIMENT
The study was performed using a custom-built ultrahigh
vacuum ~UHV! dc-magnetron sputtering system equipped
with a UHV-STM ~scanning tunneling microscope!. A schematic diagram of the system is shown in Fig. 1. The sputtering gun was purchased from U.S. Thin Film Product, Inc.
and has a standard circular planar magnetron as shown in the
747

J. Vac. Sci. Technol. A 14(3), May/Jun 1996

inset of Fig. 1. The Ru target ~99.95% purity! was purchased

from Puretech, Inc. All the data reported in this article were
obtained with the sputtering power regulated at 300 W
~within an accuracy of 3%!. The sputtering gases, O2 and Ar,
were 99.999% pure, and the O2 :Ar ratio was controlled using
mass flow controllers with accuracies of 1 sccm for Ar and
0.5 sccm for O2 . Mixing occurred in the gas line prior to
introduction of the mixture into the sputtering chamber
through a leak valve. During the evaluation of the hysteresis
loop, two Ar mass flows ~2 and 4 sccm! were used; the
pumping speed was adjusted to 5.3 and 25.2 l /s, respectively. During these measurements, the Ar mass flow was
kept constant and oxygen mass flow was gradually increased.
The total gas pressure was measured after the sputtering current was stabilized, usually for about 30 s.
All film depositions were conducted with an O2 :Ar51:1
and a total sputtering gas pressure of 15 mTorr. The pumping
speed was maintained at 25 l /s. The substrates used in this
study were purchased from Crystal Laboratories @Al2O3
~0001!# and Materials Technology International, Inc. @SrTiO3
~100!#. All wafers had the dimensions of 1031030.5 mm,
and at least one side of each wafer was polished. Each wafer
was cleaned consecutively with acetone in an ultrasonic bath
~for 7 min!, with methanol in an ultrasonic bath ~for 7 min!,
and then rinsed with distilled water and blown dry with N2 .
The wafer was then mounted onto a Mo sample holder using
either In or conducting Ag glue ~vacuum compatible!. The
sample was transferred into the sputtering chamber and degassed in three heating stages. The temperature was first
raised to 150 C and maintained until the chamber pressure
stabilized. The temperature was then raised to 300 C until
the chamber pressure stabilized at 531028 Torr. Finally the
sample temperature was increased to 450 C and was maintained for 3 h in O2 ~at 531026 Torr!.

0734-2101/96/14(3)/747/6/$10.00

1996 American Vacuum Society

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Wang et al.: Deposition and structure of RuO2 films

748

FIG. 1. Schematic diagram of the sputtering system. The inset is the geometry of the magnetron.

X-ray diffraction data were obtained using a Siemens

D-500 x-ray diffractometer or a Philips PW 1830 doublecrystal high resolution x-ray diffractometer ~l51.5405 !.
The film microstructure was studied with a Philips CM 30
transmission electron microscope ~TEM!. Rutherford backscattering spectrometry ~RBS! data were obtained using a
National Electrostatics Corporation ~MAS 1700! instrument
with a 4 He1 beam at energies ranging from 3.045 to 3.0852
MeV. The charge collected from each sample was 30 mC
using a beam current of 40 nA. The data were analyzed using
RUMP; purchased from Computer Graphics Service, Inc. The
resonance scattering cross section was estimated from the
partial-wave theory developed by Cameron using a scattering
angle of 164.1.13

III. RESULTS AND DISCUSSION

A. Reactive sputtering process

In reactive sputtering the relationship between sputtering

gas pressure and O2 mass flow often shows a hysteretical
behavior.11,14 Figure 2~a! displays the hysteresis loops found
in our system with Ar mass flows of 2 and 4 sccm. According
to these data and the well-established theory for reactive
sputtering,14 the surface of the Ru target was completely oxidized at an O2 flow ratio of 88% ~referred to as the transition
point T MO! for both Ar mass flows. The target surface converted back to Ru metal at the O2 flow ratios of 83% and
84% for 2 and 4 sccm of Ar, respectively. These transitions
are noticeably higher than those observed in the reactive
sputtering of insulating oxides such as Al2O3 and TiO2 .14,15
Figure 2~b! shows the relationship between target voltage
and O2 flow ratio for the Ar flow of 2 sccm. Similar behavior
was also observed for the Ar flow of 4 sccm. At a O2 flow of

FIG. 2. ~a! Reactor pressure vs O2 :Ar ratio in the entering sputtering gas. ~b!
Target voltage vs the O2 :Ar ratio for a 2 sccm flow rate of Ar.

50% the deposition rate was 5.2 /s, and V T was 425 V. At
100% O2 , these values dropped to 0.6 /s and 390 V, respectively.
We modeled our sputtering process using the method developed by Berg and co-workers.11,12 Because of the high
O2/Ar ratio, we introduced O1
2 current into the model to
account for the possible O2 ionization.15 The following equation was used to calculate the ratio of current densities of O1
2
(J O! and Ar1 ~J Ar!:

sO pO
JO
5
,
J Ar s Ar p Ar

~1!

where sO , sAr , p O , and p Ar are the corresponding impact

ionization cross sections and partial pressures, respectively.
The total ion current density was assumed constant at all O2
flow rates.11 Input to the model includes values for the sputtering yield of Ru and RuO2 with Ar1 and O1
2 . The sputtering yield of Ru by Ar1, corrected for secondary electron
Ru
/~11gRu!#, is known to be 1.0 at 450 eV.16 The
emission @S Ar
value for the sputtering yield of RuO2 by oxygen ions can be
determined from our data obtained at 100% oxygen flow
ratio using the following equation derived by Maniv and
Westwood:17
R 8 5G

S ~ V T ! W T
.
V T ~ 11 g !

~2!

J. Vac. Sci. Technol. A, Vol. 14, No. 3, May/Jun 1996

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749

Wang et al.: Deposition and structure of RuO2 films

FIG. 3. Comparison of the measured and calculated hysteresis loop for Ar

mass flow of 4 sccm.

The parameters R 8 , S(V T ), W T , V T , and g are the deposition

rate, sputtering yield, sputtering power, target voltage, and
secondary electron emission coefficient, respectively. G is a
geometric factor relating the deposition and sputtering rates
and will be a constant if the pressure is low. By comparing
the deposition rates at O2 flow ratios of 50% and 100%, the
yield SO
O/~11gO! of RuO2 for oxygen ions at the target voltage of 390 V can be determined as 0.1, where S O
O and gO are
the corresponding variables of RuO2 for oxygen ions. These
Ru
two yields were used as lower bounds for S Ar
and S O
O in our
fitting process. The other parameters used in the simulation
were the sticking coefficients of O2 on the Ru target a tm ~1!,
on the Ru substrate a sm ~1!, on the RuO2 target a t0 ~0!, and
on the RuO2 substrate a t0 ~0!. The substrate area ~including
the chamber wall! A s was 0.0883 m2. The ratio A T ~target
area!:A S was 1:45. The ratio sO/sAr was taken to be 2/7.15,18
The final values of fitting parameters were the following:
Ru
51.33,
total ion current density J i 5114 mA/cm2, S Ar
O
Ru
O
S Ar50.4, S O 50.25, and S O50.12. Figure 3 shows the results of the simulation for an Ar flow of 4 sccm.
The appearance of the transition to a fully oxidized target
surface occurs at a high oxygen flow ratio in the entering gas
mixture. There are several possible causes for this observation including a particularly slow rate of oxidation of the
ruthenium surface ~relative to the sputtering rate! and factors
that ultimately effect the discharge characteristics of the
plasma. We suggest that the former situation is unlikely because, even at O2/Ar flow ratios well below those needed to
oxidize the target surface; the films grown on the substrate
~at the conditions indicated! were stoichiometric RuO2 . Another likely outcome of a slow rate of oxidation would be an
increase in the total pressure as the flow rate of O2 is increased. None is observed, meaning that the deposited ruthenium atoms effectively getter all available O2 . We note, however, that other conditions can be chosen that ultimately lead
to oxygen-deficient films.
The plasma discharge characteristics will be affected by
the composition of the gas and the ion-induced secondary
electron emission of the target. Unfortunately, the values of
the secondary electron emission coefficients ~g! for Ru and
RuO2 are not available. For insulating compounds, such as

749

AlN and TiO2 , the values of g characteristically increase

upon changing from the metal target surface to the reacted
target surface.19 This increase is responsible for decreasing
the number of sputtering ions. In addition, as the insulating
compound forms on the target, it will screen the dc voltage
applied to the target and a floating voltage will build up and
inhibit further sputtering. These effects will allow the target
to become fully covered at a lower flow ratio of the reactive
gas. Other researchers have noted the requirement for
high-reactive-gas-flow ratios to achieve target saturation
when the compound ~e.g., indium tin oxide! is electrically
conductive.20 In these cases g i may not increase significantly
upon reaction of the metal surface.14,21
To probe the plasma properties of our system further, we
examined the target voltage (V T ) as a function of O2/Ar flow
ratio @Fig. 2~b!#. The following equation17 describes the relationship between g i , the sputtering ion current density
(J i ), and the target voltage:
W T 5 ~ 11 g i ! J i V T .

~3!

At constant power (W T ) J i or g i would have to increase to

cause the sharp drop in V T upon complete target oxidation.
This V T drop could result from an abrupt increase in J i due
to an O2 contribution as observed in other reactive sputtering depositions of metal oxides.22 Alternatively, g i could be
dependent upon the nature of the sputtering ion ~Ar1 vs O1
2!
~Ref. 23! which changes dramatically in the region of the
hysteresis loop. Calculations using the above model suggested that at a flow ratio of 80% O2 ~below the hysteresis
loop! Ar1 represented 99% of the total ion density. By 90%
O2 , Ar1 represented only 31.4% of the total ion density. In
the absence of further experiments, we cannot assign the
specific cause responsible for the abrupt drop in V T .
The gradual increase in V T as the O2/Ar flow ratio increases up to 88% suggested an opposite V T trend as for that
produced by a big increase of the target g i . This increase is
therefore attributed to the smaller values of J i caused by the
increasing percentage of O2 in the gas mixture coupled with
the smaller impact ionization cross section of O2 compared
to Ar.
B. RuO2 deposition on Al2O3 (0001)

All films discussed in this article were deposited using

50% O2 in the sputtering gas, a point below the hysteresis
loop. The film composition was studied using resonanceenhanced RBS.24 Figure 4 displays the results obtained from
analysis of the films deposited at 450 C for beam energies
equal to or slightly larger than the oxygen resonance energy
of 3.045 MeV.13 A uniform Ru:O ratio of 1:1.97 was observed throughout the film except in a small region close to
the film surface. The composition of the films deposited at
room temperature had the Ru:O ratio of 1:2.08. These results
agree with expected stoichiometry.
In previous studies of TiO2 and SnO2 grown by metalorganic chemical vapor deposition ~MOCVD!,2527 the film
substrate alignment was typically rutile~100!i sapphire
~0001!, and the @001# direction of the MO2 film was parallel

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Wang et al.: Deposition and structure of RuO2 films

750

FIG. 5. X-ray diffraction pattern of a RuO2 film on sapphire ~0001! grown at

room temperature and at 450 C.

sixfold symmetric pattern, consistent with the structural

model shown in Fig. 7.28
The rocking curve of the 200RuO2 reflection showed a full
width at half-maximum ~FWHM! of 0.035 compared to a

FIG. 4. RBS spectra of ~a! oxygen ~resonance-enhanced!, and ~b! ruthenium

determined at several 4 He1 beam energies.

to one of the three possible ^ 1 010& directions of the substrate. This alignment produced a threefold mosaiclike crystal structure for the film. Figure 5 shows the x-ray diffraction
data ~u 2u scan! of RuO2 films deposited at room temperature and at 450 C. The film deposited at room temperature
was amorphous, whereas the diffraction of the film deposited
at 450 C exhibited a peak at 40.572 ~the more accurate
position was determined by high-resolution x-ray diffraction!. The second film peak is the higher order reflection of
the first. Figure 6 is a plane-view bright-field ~BF! TEM
micrograph and the corresponding selected-area diffraction
~SAD! pattern. The film consists of grains of rectangular
shape that are aligned in three different directions intersecting at an angle of 120. This threefold mosaiclike structure is
similar to that found in other metal dioxide films grown on
sapphire ~0001!. The SAD pattern can be indexed using the
structural model shown in Fig. 7.26,27 The streaking property
of the diffraction spots is due to the small size of the grains.
From the relationship between the BF image and SAD pattern, we can determine that the long direction of each rectangular grain lies along RuO2 @010# direction. This direction
is parallel to one of the three ^ 2 110& directions of the substrate as seen in Fig. 6. Pole figure analysis also revealed a

FIG. 6. Plane-view bright field image of RuO2 film on Al2O3 ~0001!. The
inset is the corresponding selected area diffraction pattern.

J. Vac. Sci. Technol. A, Vol. 14, No. 3, May/Jun 1996

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Wang et al.: Deposition and structure of RuO2 films

751

FIG. 8. X-ray diffraction of the RuO2 film deposited on SrTiO3 ~100! at

room temperature and 450 C. Highly oriented film was observed in the film
deposited at elevated temperature.

that, as the lattice mismatch increases, the grain size in that

direction decreases. This is consistent with the results found
for the MOCVD of SnO2 on sapphire ~0001! substrate.25
C. RuO2 deposition on SrTiO3 (100)
FIG. 7. The structure models of ~a! sapphire ~0001! plane; ~b! the unit cell of
RuO2 and the ~100! plane structure. The oxygen height positions are relative
to the Ru positions; ~c! the epitaxial relationship.

FWHM of 0.007 for the 0006sapphire reflection. The 2u value

~40.572! of the 200RuO2 peak is, however, significantly different from that of the bulk 200RuO2 reflection ~40.021!, and
it corresponds to the lattice constant a @ 100# of 4.44 . If the
film retains a tetragonal structure, the a @ 010# will also be 4.44
. This value, however, is shifting away from both the bulk
value of a ~4.4994 ! in RuO2 and the value of 4.758
~along the [2 110] direction! of the sapphire substrate. This
scenario seems unlikely. From elastic theory,29 the shrinking
along the @100# direction should result from the elongation in
one or both of the other directions. To probe this, we estimated the in-plane lattice parameters using data from electron and x-ray diffraction studies. From the SAD pattern, the
ratio d @ 020# /d @ 01 1 # was measured to be 0.895. Assuming the
volume of the lattice unit cell does not change from its bulk
value, a @ 010# and c @ 001# can be calculated to be 4.59 and 3.09
, respectively. These values lie between the bulk RuO2 parameters and the repeat distances along the corresponding
directions on the sapphire ~0001! substrate ~Fig. 7!.
The grain lengths and the length-to-width ratio (l/w)
were measured for over 500 grains in TEM images. The
majority of the grain sizes falls into the range of 260680 .
The most frequent value of l/w is 2.4, and the average value
is 3.0. The lattice mismatch D between the film and substrate
was
estimated
for
these
two
directions
by
~d film2d substrate!/d substrate . They are D @ 010# 5 23.5%, D @ 001#
5 12.4%. The absolute value of the ratio D @ 001# /D @ 010# is 3.5,
close to the average ratio of l/w ~3.0!. This relation suggests

Figure 8 shows the x-ray diffraction data ~u 2u scan! of a

film deposited on SrTiO3 ~100! at room temperature and at
450 C. The film deposited at room temperature was amorphous, whereas the film deposited at 450 C showed only the
200RuO2 reflection. The out-of-plane film orientation is thus
~100!RuO2iSrTiO3 ~100!. The plane view BF TEM image
did not show in-plane alignment, presumably because of
large lattice mismatch ~at least 12.6%! between RuO2 and
SrTiO3 ~100!.
IV. CONCLUSIONS
Increasing the percentage of oxygen in the entering sputtering gas mixture causes a transition on the target from a
metallic to a metal oxide surface at 88% O2 . Upon lowering
the percentage of O2 the target returns to a metal surface
around 82% 84% depending on the mass flow of Ar. Compared to the reactive sputtering of insulating metal oxides,
the higher values of the O2/Ar required to observe the characteristic hysteresis loop was attributed to the excellent metallic conductivity of RuO2 . High metallic conductivity of
RuO2 reduces the difference in the efficiency of secondary
electron emission between Ru and RuO2 and allows a finite
sputtering rate of the compound itself. For insulating metal
oxides, the normally higher value of the secondary electron
emission coefficient is one of the important factors which
reduces the ion current and, therefore, the sputtering rate
compared to the oxide-free metal surface.
Films deposited at room temperature were amorphous regardless of the type of substrate, whereas films grown at a
substrate temperature of 450 C were crystalline. On SrTiO3
~100! an oriented polycrystalline film was produced with the
RuO2 ~100! face parallel to the substrate. The RuO2 ~100!
face was the only orientation observed on Al2O3 ~0001!. In-

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Wang et al.: Deposition and structure of RuO2 films

plane alignment of the @001# RuO2 direction with the three

^ 1 010& substrate directions resulted in a threefold mosaic
microstructure.
ACKNOWLEDGMENTS
The authors would like to thank Dr. Donald McClure at
3M for valuable discussions, and Dr. Xiaofeng Zheng at Argonne National Laboratory for obtaining some of the transmission electron micrographs. This research was supported
by the Center for Interfacial Engineering, a National Science
Foundation funded Engineering Research Center at the University of Minnesota.
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