Improvements of the SiC Homoepitaxy Process in a

Journal
of Electronic
Materials, Vol.
28, No.
3, 1999
Horizontal
Cold-Wall
CVD
Reactor

Special Issue Paper

175

Improvements of the SiC Homoepitaxy Process in a

Horizontal Cold-Wall CVD Reactor
F. WISCHMEYER,1,3 E. NIEMANN,1 and H.L. HARTNAGEL2
1.Daimler-Benz AG, Research and Technology, FT2/EM, Goldsteinstr. 235, D-60528 Frankfurt,
Germany. 2.Technical University Darmstadt, Institut fr Hochfrequenztechnik, Merckstr. 25,
D-64283 Darmstadt, Germany. 3.email: frank.wischmeyer@dbag.fra.daimlerbenz.com

In this research effort, we investigate the influence of the cold-wall reactor

geometry on the chemical vapor deposition (CVD) growth process of 4H-SiC and
the quality of lightly doped epitaxial layers. Stable growth conditions with
respect to growth rate and C/Si ratio of the gas-phase can be achieved by the
appropriate choice of the distance between susceptor and walls of the inner
quartz tube. A background doping concentration in the range of 1014 cm3 is
realized by employing a high temperature stable and hydrogen etch resistant
coating of the graphite susceptor. Doping and thickness homogeneity of epitaxial
layers on 35 mm diam. 4H-SiC substrates, expressed by /mean, are as low as
6.9 and 7.7%, respectively. From deep level transient spectroscopy measurements, the concentration of the frequently reported intrinsic Z1-center in 4H-SiC
is determined to be below the detection limit of 1012 cm3.
Key words: Chemical vapor deposition (CVD), deep level transient
spectroscopy (DLTS), doping, homogeneity, horizontal reactor,
purity, SiC

INTRODUCTION
Silicon carbide (SiC) is a wide bandgap semiconductor with a high potential to be used for diodes and
discrete power devices similar to Si-isolated gate
bipolar transistors (IGBTs), particulary in converter
systems. There is a strong advantage for SiC electronics in applications for high temperature and high
frequency devices. In SiC, the on-state and switching
losses are drastically reduced. The decreased on-state
losses result from a lower on-resistance of SiC devices, because the allowed doping level needed for a
certain blocking voltage is higher, due to the critical
electrical field in SiC, which is about one order of
magnitude higher than in Si devices.
Low switching losses are a characteristic of unipolar devices (Schottky-diodes and field effect transistors [FETs]). Using SiC, these properties can be extended to very high voltages (> 2000 V). Electrical
power systems based on SiC devices lead to a clear
reduction of the cooling requirements. Moreover, the
unipolar SiC devices yield improved switching speed.
Therefore, SiC devices can be operated at higher
frequencies, which offers the possibility to use smaller
passive components.
This means, that very compact, light and efficient
electrical power distribution units can be built for all
(Received August 4, 1998; accepted November 6, 1998)

mobile systems. Consumer electronics (like power

factor control modules) and industrial applications
are another promising field of application for SiC
devices. Due to the lower intrinsic carrier concentration, SiC can also be operated at high temperatures of
up to 600C.
A good crystal quality of SiC is important to
manufacture SiC devices with the desired performance. Within almost all diode and transistor concepts, the epitaxial layer plays a crucial role. Therefore, high quality epitaxial SiC layers will pave the
way to optimally operating devices.
Chemical vapor deposition (CVD) growth of electrically active SiC epitaxial layers is widely recognized as the technology of choice to fabricate lightly
doped material with reasonable growth rates. For
several reactor concepts like hot-wall CVD,1 vertical
cold-wall CVD,2 and CVD in a horizontal multiwafer
reactor3 (both latter examples employ substrate rotation), the realization of high quality silicon carbide
material has been reported. Silane and propane diluted in a hydrogen carrier gas flow are typically used
as source gases.
In CVD, the homogeneity of epitaxial layers with
respect to growth rate and doping concentration often
suffer from depletion of reactants along the susceptor
and reactor walls. Therefore, we have investigated
the influence of the reactor geometry on the homogeneity and quality of epitaxial 4H-SiC layers for a
175

176

Wischmeyer, Niemann, and Hartnagel

Fig. 1. Cross section of the modified quartz liner tube. The dashed line
marks the shape of the standard liner.

Fig. 2. Surface temperature profile of a 35 mm diameter substrate at

the growth temperature.

single wafer horizontal cold-wall CVD system in conjunction with the feature of an inductively heated
rotating susceptor.
EXPERIMENTAL
Based on a commercial CVD system,4 customer
specific modifications have been made to overcome
strong reactant depletion at the quartz walls of the
inner quartz liner tube. Due to an excessive heat
radiation of the 108 mm diameter disk-like susceptor,
the ceiling of the quartz tube reaches temperatures
about 1000C, which leads to an undesired deposition
of silicon at the tube ceiling during SiC growth. With
increasing thickness even more energy is absorbed by
the film and finally the main deposition takes place at
the upper reactor wall. Choosing an appropriate liner
tube profile the co-deposition at the ceiling can be
suppressed totally for typical growth temperatures
between 1400 and 1500C, as can be seen in Fig. 1.
This design appears to be a good compromise between
maximizing the distance between susceptor and tube
walls and the ability to maintain a laminar gas flow

pattern, as will be discussed later. As another benefit

of the modified liner, temperature control of the
process via pyrometrical measurement of the SiC
substrate surface is possible. This in-situ monitoring
eliminates the error of temperature uncertainties due
to changes of the emissivity of the susceptor surface
during SiC deposition.
In a horizontal reactor geometry, great attention
has to be paid to a suitable coating of the hot graphite
parts. Since the main gas stream passes over the hot
susceptor surface, breakage or degradation of the
coating will result in a change of the carbon to silicon
(C/Si) ratio in the gas composition due to free hydrocarbons released from the graphite.5 Additionally,
impurities like B and Al from the graphite will cause
a high compensating background impurity level.6
Usually, SiC is used as coating material, having the
great disadvantage of being rapidly etched by the
hydrogen at hot spots where no SiC deposition takes
place. Furthermore, the part of the susceptor coating
underneath the SiC substrate shows strong sublimation of the coating material. After the growth experiment, a polycrystalline SiC deposit can be found on
the wafer backside, as it is colder than the susceptor
surface due to the non-ideal thermal contact. These
two effects strongly limit the lifetime of SiC coated
susceptors.
The use of a high temperature stable and hydrogen etch resistant coating material of the graphite
susceptors has led to a prolonged lifetime and to a
reduction of the unintentional doping background in
our system from 1016 to the range of 1014 cm3. When
using a coating material different from SiC, an emissivity change of the susceptor surface during SiC
deposition has to be compensated for by adjusting the
radio frequency (rf)-power of the inductive heating.
Because of the above mentioned possibility of measuring the SiC substrate temperature during the
entire process, this change of emissivity can be automatically compensated for, thereby holding the substrate temperature at a constant value.
By optimizing the shape of the rotating susceptor,
a good temperature homogeneity across 35 mm diameter SiC substrates has been achieved. Figure 2 shows
a typical substrate temperature profile with a total
temperature deviation of less than 1% at the growth
temperature of 1450C.
The substrates used in this study are 4H-SiC
(0001), Si-face, 8 off-axis toward [11 2 0] from Cree
Research Inc., Durham NC, USA.
For electrical characterization of the epitaxial
layers titanium (Ti) Schottky-diodes have been fabricated by sputtering on the as-grown epitaxial side of
the wafer. The photolithographic structuring of the
contacts allows an exact measure of the diode area. Ti
sputtered onto the polished backside of the wafer
serves as large ohmic backside contact. Capacitance/
voltage measurements have been carried out to determine both the net donor concentration and the thickness of the epitaxial layer. In addition, deep level
transient spectroscopy has been performed to investi-

Improvements of the SiC Homoepitaxy Process in a

Horizontal Cold-Wall CVD Reactor

gate electrically active defects of the grown material.

RESULTS AND DISCUSSION
Growth Rate
Because of the strong influence of fluid flow phenomena on film thickness and uniformity, the maintenance of a laminar flow pattern for the increased
reactor diameter is important. Flow visualization
experiments have been undertaken by saturating the
hydrogen carrier gas with silane. For certain critical
concentrations (depending on total flow rate, temperature and total reactor pressure), Si clusters or
particles 2,7 are formed in the gas-stream which reflect
the light from the glowing susceptor. In this way, the
gas flow pattern above the susceptor can be investigated easily and the basic growth parameters can be

177

optimized. As experimentally optimized parameters,

a total flow rate in the range of 1214 slm and a
reduced total reactor pressure between 150 and 250
mbar have been deduced.
The linear dependence of the growth rate from the
pure SiH4 flow is shown in Fig. 3. Reasonable growth
rates up to 3 m/h can be achieved. The time dependence of the growth rate given in Fig. 4 is constant,
demonstrating the stable growth conditions realized
with the modified reactor geometry.
Doping
The investigations of intentional incorporation of
dopants into SiC have been concentrated on nitrogen
(N2) as dopant source for n-type conductivity epitaxial
layers. For three different N2 flows, the C/Si ratio of
the source gases have been varied. In accordance with
the site-competition effect,8 nitrogen can be prevented

Fig. 3. SiH4 dependence of the growth rate.

Fig. 5. C/Si ratio dependence of the doping concentration.

Fig. 4. Time dependence of the growth rate.

Fig. 6. Nitrogen flow dependence of the doping concentration.

178

Wischmeyer, Niemann, and Hartnagel

Fig. 7. Map of the doping homogeneity of an epitaxial layer across a

35 mm substrate.
Fig. 9. DLTS spectrum of an n-type 6 1015 cm3 doped 4H-SiC
epitaxial layer for a rate windows of t1/t2 = 1 ms/2 ms.

Fig. 8. Map of the thickness homogeneity of an epitaxial layer across

a 35 mm substrate.

from incorporating into the layer by increasing the

C/Si ratio, as shown in Fig. 5. In contrast to growth
experiments with the standard liner tube (denoted as
warm wall), this obvious sensitivity of the donor
concentration to an increased carbon supply demonstrates that the gas-phase composition is not influenced by either a severe depletion of Si at the reactor
walls or an excess supply of hydrocarbons from the
graphite parts, which represent two major reasons
causing a carbon rich atmosphere above the substrate.
In Fig. 6 the nitrogen flow dependence of the net
donor concentration for similar effective C/Si ratios is
given. For both reactor geometries, the incorporation
efficiency of nitrogen remains unchanged.
Homogeneity
For device applications, the lateral homogeneity of
doping distribution and thickness of the epitaxial
layers are of great importance. A map of the variation

of these two SiC film properties is determined by

capacitance-voltage (C-V) measurements on a densely
arranged array of Schottky-diodes. Figure 7 shows a
map of the net donor concentration of a nitrogendoped epitaxial 4H-SiC layer. Over the entire 35 mm
diameter wafer, a doping concentration variation
expressed by the standard deviation /mean = 6.9%
can be extracted. Excluding about 4 mm of the wafer
edge, this value is reduced to 4.6%. In this specific
case, the slight asymmetry in the doping distribution
is most likely caused by a better temperature coupling
of the upper right edge of the wafer to the susceptor.
The thickness variation of the epitaxial layer is
given in Fig. 8. The deviation of the layer thickness
over the total wafer is /mean = 7.7%. Again, excluding the wafer edge, this value decreases to 4.4%. A
slight depletion of reactants along the susceptor most
likely causes the reduction of the layer thickness
toward the center of the wafer. The clear rotation
symmetrical thickness profile demonstrates the beneficial influence of the substrate rotation.
Electrically Active Defects
In order to investigate electrically active defects in
the material, deep level transient spectroscopy (DLTS)
measurements have been obtained from Ti-4H-SiC
Schottky-diodes. The DLTS spectrum for a rate window of t1/t2 = 1 ms/2 ms is plotted in Fig. 9. In the
examined temperature range above 100K, only one
peak (denoted with 1) can be found with an activation
energy of 390 meV assuming T 0. The concentration
of the center is determined to N(1) = 5.7 1012 cm3.
The nature of this peak is unknown. The slight increase in the spectrum for temperatures above 550K
is attributed to an increase of the diode leakage
current.
A frequently reported intrinsic defect in highquality as-grown 4H-SiC epitaxial layers is the Z1

Improvements of the SiC Homoepitaxy Process in a

Horizontal Cold-Wall CVD Reactor

center with an activation energy of 610 to 670 meV.9

Typical concentrations of about N(Z1) = 1013 cm3 are
given.9,10 From the DLTS spectrum in Fig. 9, it can be
seen that the concentration of the intrinsic Z1 center
is below 1012 cm3, which is the resolution limit of this
measurement mainly determined by the diode leakage current and the noise of the capacitance measurement setup. This excellent value demonstrates the
achieved high-quality of the 4H-SiC epitaxial layer.
CONCLUSIONS
Geometry changes of the inner quartz tube of the
horizontal cold-wall CVD reactor lead to a temperature controlled SiC growth process, that is stable with
respect to growth rate and C/Si ratio of the gas-phase.
A reduction of the background doping concentration
to a level of 1014 cm 3 is achieved by employing a high
temperature stable, hydrogen etch resistant coating
of the graphite susceptor.
By varying the nitrogen flow and/or the C/Si ratio
of the source gases, a net donor doping concentration
of epitaxial layers between 1015 and 1018 cm3 can be
obtained.
The benefit of a rotating susceptor in a horizontal
reactor geometry is clearly demonstrated by the maps
of donor concentration and epitaxial layer thickness.
Slight depletion effects are leveled out and for both of
these layer properties /mean values below 5% can be
achieved for the center part of 35 mm diameter substrates. The excellent quality of the epitaxial 4H-SiC

179

layers is demonstrated by DLTS measurements. The

concentration of the intrinsic Z1 center, which is a
commonly observed defect in 4H-SiC epitaxial layers, is
determined to be below the detection limit of 1012 cm3.
ACKNOWLEDGMENTS
The authors would like to thank Dr. G. Pensl and
Mr. M. Weidner, U. Erlangen, for performing and
analyzing the DLTS measurement. The support of
Dr. H. Jrgensen and Mr. J. Kppeler, Aixtron AG,
Aachen, is gratefully acknowledged.
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