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Defect structure of epitaxial GaN

films determined by transmission
electron microscopy and triple-axis
X-ray diffractometry
a a a b
T. Metzger , R. Höpler , E. Born , O. Ambacher , M.
b c c c
Stutzmann , R. Stömmer , M. Schuster , H. Göbel , S.
d d d
Christiansen , M. Albrecht & H. P. Strunk
a
TU-München, Institut für Mineralogie and Geochemie ,
Lichtenbergstr. 4, D-85748, Garching, Germany
b
Walter Schottky Institut , D-85748, TU-Müchen, Am
Coulombwall, Garching, Germany
c
Siemens AG, Otto-Hahn-Ring 6 , D-81739, München,
Germany
d
Universität Erlangen-Nürnberg, Institut für
Werkstoffwissenschaften-Mikrocharakterisierung , Cauerstr.
6, D-91058, Erlangen, Germany
Published online: 12 Aug 2009.

To cite this article: T. Metzger , R. Höpler , E. Born , O. Ambacher , M. Stutzmann , R.

Stömmer , M. Schuster , H. Göbel , S. Christiansen , M. Albrecht & H. P. Strunk (1998)
Defect structure of epitaxial GaN films determined by transmission electron microscopy
and triple-axis X-ray diffractometry, Philosophical Magazine A, 77:4, 1013-1025, DOI:
10.1080/01418619808221225

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 PHILOSOPHICAL A, 1998, VOL.77, No. 4, 1013-1025
MAGAZINE

Defect structure of epitaxial GaN films determined by

transmission electron microscopy and triple-axis X-ray
diffractometry

By T. METZGER,
R. HOPLER,E. BORN
TU-Munchen, Institut fur Mineralogie and Geochemie, Lichtenbergstr. 4,
D-85748 Garching, Germany

0.AMBACHER,
M. STUTZMANN
Downloaded by [Indian Institute of Science] at 06:11 13 February 2015

Walter Schottky Institut, TU-Muchen, Am Coulombwall, D-85748 Garching,

Germany

R. STOMMER,
M. SCHUSTER,
H. GOBEL
Siemens AG, Otto-Hahn-Ring 6, D-81739 Munchen, Germany

M. ALBRECHT
S. CHRISTIANSEN, and H. P. STRUNK
Universitat Erlangen-Nurnberg, Institut fur Werkstoffwissenschaften-
Mikrocharakterisierung, Cauerstr. 6 , D-91058 Erlangen, Germany

[Received 25 February 1997 and revised version accepted 3 August 1997

ABSTRACT
Important structural characteristics (correlation lengths of columnar
crystallites, dislocation densities, angles of rotational disorder) of hexagonal
GaN grown by metallorganic chemical vapour deposition on c-plane sapphire
are determined by transmission electron microscopy and triple-axis X-ray
diffractometry. GaN films exhibit an edge dislocation density in the range of
10" cm-', a tilt and twist angle of 0.1" and 1.3" and a columnar structure with
a lateral and vertical correlation length of 150 and lOOOnm respectively. The
determination of correlation lengths and dislocation densities from X-ray
patterns was undertaken using two independent evaluation methods which are
discussed in detail. It is also shown that triple-axis X-ray diffractometry is a highly
suitable technique for the separation of different kinds of structural defects such
as edge and screw dislocations that lead to a characteristic broadening of
symmetric and asymmetric Bragg reflections. The correlation lengths and
dislocation densities are obtained additionally by electron transmission
microscope investigations which are in good agreement with the X-ray
diffraction results.

8 1. INTRODUCTION
State of the art epitaxial layers of G r oup I11 nitrides that are intended for use in
electronic and optoelectronic devices exhibit a high density of structural defects
compared with other 111-V epitaxial systems such as GaAs o r InP. High dislocation
densities, mosaicity, tilted and twisted small crystallites are well known character-
istics of the heteroepitaxial layers of G r oup 111 nitrides (Lester et al. 1995, Ning et al.
1996). Dislocation densities up t o 10" cmP2 are common in GaN-based heterostruc-
tures and high efficiency blue light-emitting diodes (Lester et al. 1995). These defects
0141-8610/98 $12 00 0 1998 Taylor & Francis Ltd
 1014 T. Metzger et al.

lead to observable effects in the films, which are often analysed by X-ray diffraction
(XRD) techniques. In particular, the measurement of the full width at half maximum
(FWHM) of the rocking curve with a double-crystal diffractometer is a well estab-
lished method of proving the epitaxial quality of GaN films (Compton and Allison
1935, Matsushita et al. 1971). This method is often applied for the determination of
dislocation densities in semiconductors exhibiting cubic symmetry (Qadri and Dinan
1985, Fatemi et al. 1993, Ayers 1994). Nevertheless, application of this method in the
field of Group 111 nitrides presents some challenges because the thermodynamically
stable phase crystallizes in the wurtzite structure and one has to be aware of an
anisotropic distribution of dislocations. The broadening of the XRD curve is
affected not only by the dislocation structure. Additional various structural imper-
fections (heterogeneous strain, small correlation lengths, impurities) and instrumen-
tal broadening will influence the diffraction pattern (Hordon and Averbach 1961,
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Fatemi et al. 1993, Ayers 1994). The heterogeneous strain, the correlation lengths
normal and parallel to the substrate surface and the degree of mosaicity expressed by
the tilt and twist angles are key issues in characterizing the quality of epitaxial films
with a large lattice mismatch to the substrate.
The aim of this study is the determination of the characterizing structural fea-
tures (heterogeneous strain, correlation lengths normal and parallel to the substrate
surface, tilt and twist) and dislocation densities (edge and screw dislocations) of
hexagonal epitaxial G a N films. We show how the XRD technique using a triple-
axis diffractometer can be applied to determine structural quality by measuring
several Bragg reflections in different scan directions.
Additionally, transmission electron microscopy (TEM) measurements are per-
formed in order to obtain detailed knowledge of the defect structure present in the
sample investigated by X-ray diffraction, because a direct image of structural defects
is produced. Furthermore, this procedure is useful for the determination of disloca-
tion densities by XRD, where the Burgers vector, slip plane and line direction of
dislocations has to be known. Furthermore, TEM is used as a reliable cross-check of
the results obtained by XRD.

$ 2 . EXPERIMENT A N D THEORY
We deposited epitaxial GaN films on (0001) A1203 substrates by metallorganic
chemical vapour deposition (MOCVD) using the reaction of triethylgallium (Et3Ga)
with ammonia (NH3) in the presence of nitrogen (N2) and hydrogen (Hz). The flow
rates of NH3 N2 and HI were maintained at 33, 16 and 16 mbar 1 s-’ respectively,
producing a gas velocity of 50 cm sC1in the horizontal, home-made MOCVD system
at the substrate position. The Et3Ga flux was fixed at 2.2 pmol min-’, which caused a
growth rate of 0.7 pm h-’ at a pressure in the deposition chamber of 100 mbar. First
a low temperature GaN buffer layer of thickness of 50 nm was grown at 530°C. The
growth temperature was raised then to 950°C and 1 pm thick epitaxial films were
grown (Ambacher et al. 1997).
The films exhibited a smooth surface with a root mean square surface roughness
of 2 nm determined by atomic force microscopy (Digital Instruments Nanoscope
IIIa). The concentration of free carriers and their mobility (n, M 2 x 10l6~ m - ~ ,
pe M 200 cm2 V s-I) were determined by Hall measurements. The near bandgap
photoluminescence measured at 4 K had a peak position of 3.476eV and a
FWHM below 1OmeV.
 Defects in epitaxial GaNfilms 1015

The X-ray measurements were performed on two different triple-axis diffract-

ometers: (i) a Philips Xpert MRD triple-axis diffractometer equipped with a four-
bounce Ge(022) monochromator and a three-bounce Ge(022) analyser crystal using
CUKEradiation from a 2.2kW ceramic tube, reaching a resolution limit of about
10arcsec; and (ii) a Siemens D5000 high resolution diffractometer equipped with a
curved graded multilayer and an eight-bounce Ge(022) monochromator as primary
optics and a multilayer mirror as secondary optics. The first mirror acts as a con-
densor for the divergent X-ray beam emanating from the source (1.5 kW Cu anode).
With this optical element, parallel beam coupling of a highly intense X-ray beam into
the monochromator crystal is attained (Schuster and Gobel 1995, 1996).
The TEM measurements were performed in a Philips CM30 and a Philips
CM300UT microscope, both operating at 300 kV, with which a resolution of
0.165 nm was achievable.
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2.1. Results of transmission electron microscopy measurements

An example of the TEM diffraction contrast analysis of the defect structure is
shown in figure 1 ( a t ( c ) .The majority of the threading dislocations are in the [OOOIJ
line direction, i.e. they lie along the surface normal. They have Burgers vectors
b, = f (1120), b, = [OOOl] and bcfa= i(1123) (in the following called a-, c- and
c + a-type dislocations respectively). From the line direction and the Burgers vector
we obtain the glide plane and the character of the dislocations: a-type threading
disIocations thus are pure edge dislocation and have a (1TOO) glide plane, c-type
dislocations are pure screw dislocations, while c + a-type dislocations are of mixed
type. The predominant defects in our samples are a-type dislocations (pure edge
dislocations) that are present with a density in the range of 10"cm-2. From a
corresponding analysis of plan view micrographs (figure 2 (a)) we note that some
of these dislocations are arranged in the form of small angle grain boundaries in
( 1 TOO) planes. A high resolution micrograph taken along the [000 11 projection of a

Figure 1. Dislocation distribution in GaN/A1203 (000 I), contrast analysis. TEM, weak-
beam dark-field conditions. (a) Only dislocations that have an a-type Burgers vector
component are visible under the chosen imaging conditions. (b) Only dislocations with
a c-type Burgers vector component are visible. (c) Small angle grain boundaries
(marked by arrows) lie obliquely in the volume of the layer.
 1016 T. Metzger et al.
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Figure 2. Small angle grain boundaries in GaN/AI2O3(OOOI), consisting of pure edge type
dislocations. The correlation length obtained from the spacing of these grain bound-
aries is 150-250nm. (a) Transmission electron micrograph in plan view under weak-
beam dark-field conditions,(b) Plan view high resolution TEM image of pure edge
dislocations with b, = f(l120) and line direction I = [OOOI].

single dislocation is shown in figure 2(b). The small angle grain boundaries can be
seen in figure 1 (c) as dislocation walls lying obliquely in the volume of the sample.
These small angle grain boundaries mediate a twist around the [OOOl] surface nor-
mals of the adjacent crystallites (Ponce 1997). The correlation length of the crystal-
lites obtained from the average spacing of the small angle grain boundaries (figure
2 (a)) is 150-250 nm. c-Type threading dislocations (Burgers vector b = [OOOl])occur
in a significantly lower density of about 8 x 10' cmP2 compared with the pure edge
dislocations. c + a-type dislocations appear with a very low density (less than
lo8cmp2). Planar defects such as stacking faults, inversion domain boundaries and
Frank partial loops, parallel and perpendicular to the surface, could not be observed
in the investigated GaN films.
 Defects in epitaxial GaNJilms 1017

2.2. Theory of X-ray diffraclion measurements

Using a triple-axis diffractometer for the measurements, the broadening of the
rocking curve (angular-scan or Q-scan) of the symmetric reflections 0002, 0004 and
0006 of GaN grown on c-plane sapphire is influenced only by the tilt (out-of-plane
misorientation) and the small correlation length parallel to the substrate surface.
Wafer bending or heterogeneous strain do not influence the peak broadening owing
to the small acceptance angle of the detector. As the broadening in reciprocal space
due to tilted crystallites is proportional to the scattering order and the broadening in
reciprocal space due to a small correlation length is independent of the scattering
vector, a graphical separation of these two effects is possible by recording higher
order reflections. If a linear supposition of both effects is assumed, a separation
analogous to the Williamson-Hall (1953) plot can be performed, when
PQ(sin@)/A is plotted against (sin @)/A for each reflection and fitted by a straight
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line. PQis the integral width of the measured profile, A is the X-ray wavelength and
2 0 is the scattering angle. From the y-intersection yo of the fitted line the correlation
length LIIcan be estimated (LII= 0.9/(2y0)). The slope is a direct measure of the tilt
angle aQ.A second analytical method is based on the assumption that small correla-
tion lengths lead to a Cauchy profile whereas tilted growth results in a Gaussian peak
shape (Gay et al. 1953, Schoening 1965, De Keijser et al. 1983).
The convolution of a Gaussian G ( x ) and a Cauchy profile C(x) is called a Voigt
(191 2) function, which can be approximated by a pseudo-Voigt function P ( x ) :
P ( x ) = Z O [ r l C ( X ) + (1 - Q)G(X)l 0677<1, (1)
with Zo as a scaling factor. Determining the parameter Q of the pseudo-Voigt function
by a least squares fit and knowing the integral width ,BQof the fit, one can calculate
the lateral correlation length LIIand the tilt angle an considering the formulae given
by De Keijser et al. (1983):
0.9A
+ sin@ ’
Lli = pQ(0.017475 1.500484~- 0.534156~~)

(E@ = &[0.184446 + 0.812692(1 - 0.998497~)”~0.65960377 + 0.4455477’1.

- (2b)
If one assumes that both screw dislocations (b = [OOOl])are related to an edge-
type misfit dislocation in the interface with the same Burgers vector that leads to a
corresponding tilt of single crystallites, the density of these screw dislocations N,ooo,~
can be obtained using the following equation of Gay, Hirsch and Kelly (1953) and
modified by Dunn and Koch (1957):

where b, is the Burgers vector of the c-type threading dislocation (lb,l = 0.5185 nm).
In the radial-scan direction (2O-Q-scan) of the symmetric reflections 0002, 0004
and 0006, a small correlation length normal to the substrate surface and a hetero-
geneous strain along the c-axis causes a broadening of the Bragg reflections. Again
these two effects can be separated owing to either their different dependency on the
diffraction vector (Williamson-Hall (1953) plot) or to their different effects on the
peak shape (Cauchy profile for a small correlation length, Gaussian profile for
heterogeneous strain (De Keijser et al. 1983)). In the Williamson-Hall plot,
P28-0(c0s @)/A is plotted against (sin @)/A for each reflection and again fitted by
 1018 T. Metzger et al.

a straight line. From the y-intersection yo the correlation length L L can be estimated
( L , = 0.9/(2y0)) and the strain E, is obtained directly from the slope of the line
which is 4 ~Using ~ .the integral width P2@-@and the parameter Q of the least squares
fit with a pseudo-Voigt function performed on a single reflection, the correlation
length L , and the strain normal to the substrate surface E~ can be obtained from the
equations given by Scherrer (1918), Stokes and Wilson (1944) and De Keijser et al.
(1983):
0.9X
LI =
&8-0(0.017475 + 1.500484~ 0 . 5 3 4 1 5 6 ~cos
- ~) 0 ’

E l =
&-o[0.184446 + 0.8 l2692( 1 0.998497q)’” 0.659603~+ 0.445542~~1
- -

4 tan 0
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It should be mentioned that another method which can be used to separate strain
and size effects on the peak broadening is the Warren-Averbach analysis (Hordon
and Averbach 1961, Warren 1969). However, such an analysis was not used in this
study.
a-Type threading dislocations (b, = (1 lZ0)) mediate an azimuthal rotation of
crystallites around the surface normal. This twist angle C Y ~can be measured by
performing @-scanson asymmetric reflections (surface normal and diffraction vector
are not parallel), where the sample is rotated with respect to the surface normal.
From the measured broadening /3@of the @-scans,the dislocation density N E can be
derived using the equation of Gay et al. (1953), modified by Dunn and Koch (1957),
when the broadening due to small correlation lengths Llican be neglected (&, = a@):

where bE is the Burgers vector of the edge dislocations. (In our case
IbE)= Ib,l = 0.3189 nm.) This equation holds only for a strictly random distribution
of dislocations. If dislocations are piled up in small angle grain boundaries, the
following formula is used (Fewster 1989), which describes the formation of subgrains
with an average size L11. where a: is again the twist angle:

For a system with both dislocation distributions (randomly and piled up), as
observed in the GaN sample, the real dislocation density will lie between these
two values.
As mentioned above, from the broadening of 0001 reflections in the radial-scan
direction, the heterogeneous strain E~ can be obtained. Considering that each dis-
location is accompanied by a strain field, it is possible to calculate the dislocation
density also from the strain broadening $
’!, of Bragg reflections in the radial direction
using the following equations (Fewster 1989). provided that the slip planes and
Burgers vectors of the dislocations are known.

,!?: = 8(~’)(1n2)tan2@. (7)

 Defects in epitaxial GaNJilms 1019

( E ~ is
) the mean square strain and can be calculated for a pure screw dislocation by
(Stehle and Seeger 1956, Fewster 1989):

Y s is the angle between the Burgers vector bs and the normal of the diffracting
lattice plane and rs and ro are the upper and lower integration limits of the strain
field respectively. For ro, a value of 10p7cm is assumed (Qadri and Dinan 1985,
Fewster 1989) and rs is related to the screw dislocation density Ns by:
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From eqn. (8) it is obvious that 0001 reflections cannot be broadened by screw
dislocations with bs = [OOOI], because in this case, Y s becomes zero. A distinct
broadening of the radial-scan direction (20-52-scan) can be expected only for asym-
metric reflections.
For the calculation of the mean square strain of edge dislocations (&), the
following equation holds (Fewster 1989):

(EE)
2 = w5b2,
ln($)f(A,Y~), , f ( d , Y ~ , ) =( ~ . ~ ~ c o s ~ A + O . ~ ~ (10)
COS~YJ=)

where bE is the Burgers vector, YE is again the angle between the Burgers vector and
the diffraction plane normal and A is the angle between the normal of the slip plane
and the normal of the diffracting plane. The edge dislocation density N E is related to

Since there are three distinct dislocation systems for pure edge dislocations in GaN,
the mean square strain (EL)is influenced by all three possible orientations. In table 1,
the angles $E and d as well as the term f ( d , YE) are summarized for the three
individual slip systems { lOT0) and the diffraction vector 1074. Corresponding values
are obtained for other asymmetric reflections. From eqn. (10) it is also clear that pure
edge threading dislocations with b, = (1 120) do not influence the symmetric 0001
reflections of GaN since the angles YE and d are both 90" and again only asymmetric
reflections are broadened in the radial-scan direction (20-52-scan) by these threading
dislocations. In order to calculate the mean square strain due to screw and edge
dislocations, the individual square strains can be summed as follows:
p,' = 8( (€2,) + (.;))(In 2) tan2 0. (12)

Table 1. Values of A , Y E and f ( d , YE)for the three

edge dislocation systems with bE = +,(1120)
and the slip planes {llOO}, (1014 reflection).

(oi10) 102.3 68.4 0.172

(ioio) 64.8 90.0 0.443
(iioo) 102.3 111.6 0.172
 1020 T. Metzger et al.

Using eqns. (8H12), the strain broadening of asymmetric reflections can be simu-
lated for different densities of screw and edge dislocations and then compared with
the measured values.

$ 3 . RESULTSAND DISCUSSION
For all the measured reflections, a correction for the instrumental broadening
and the intrinsic FWHM is not necessary because these effects are very small (only a
few arcsec) compared with the measured broadening due to crystal imperfections.
For determination of the strain and correlation length normal to the substrate
surface, a Williamson-Hall plot for the symmetric 0002, 0004 and 0006 reflections
and the pseudo-Voigt fit were used. From the Williamson-Hall plot, the correlation
length L , cannot be deduced in a reliable way because the fitting line intersects they-
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axis near the origin, which indicates a large correlation length of the order of 1 pm.
The strain normal to the substrate E~ obtained from the slope is 3.7 x lop4.Figure 3
shows the measured profile and the pseudo-Voigt fit of the 0002 reflection of GaN
with the parameter 71 equal to 0.668. From t h s value and the integral width of
0.024", the correlation length L, was obtained (500nm) and the strain value E~
was calculated to be 1.4 x lop4 according to eqns. (4 a ) and (4 b). The discrepancy
between both methods concerning the strain value E~ can be explained as follows: in
the William-Hall plot a linear correlation between strain and size is assumed, which
is only a rough approximation (Balzar and Popovic 1996). The large correlation
lengths L , obtained by both methods were confirmed by TEM measurements indi-
cating that only the layer thickness limits the correlation length. A possible explana-
tion for the origin of the heterogeneous strain E~ is the misfit dislocations with
4
b, = (1 130) present in the film-substrate interface region. This would also explain
the decreasing broadening of the radial-scans with increasing film thickness, which
was also observed. The volume fraction of this highly defective region is reduced
with increasing layer thickness and thus the profiles are less broadened.

1.0- a) GaN 0002

T =0.668

0.0 -
E
(I)
f
c
0.6-
C

ji
0.00.2
0.2
0.1
0.1
0.0
0.0
Ma["]
0.1
0.1
0.2
0.2 4.2 0.1 0.0
Ma["]
0.1

Figure 3. Measured G a N 0002 diffraction profile (filled circles) fitted with a pseudo-Voigt
function (full curve) used for the separation of the heterogeneous strain parallel to c,
and the vertical correlation length L,: (a) linear scaling; ( h ) logarithmic scaling.
 Defects in epitaxial GaNJilms 1021

In figure 4 the values ,&(sinO)/A of the symmetric rocking curves 0002, 0004
and 0006 are plotted against (sin @)/A and fitted linearly. From the y-intersection
the lateral correlation length LIIwas estimated to be 150nm, the slope of the fit gave
a tilt angle an of 0.13", from which a dislocation density for the screw dislocations of
4.4x lo8 cm-* was obtained using eqn. (3). Pseudo-Voigt analysis (eqns. (2a) and
(2 b)) yields a correlation length parallel to the substrate LIIof 190 nm and a tilt angle
an of 0.1", from which a dislocation density of 2.6 x 1O8cmP2was derived. Both
analytical methods agree satisfactory and also show good agreement with the results
obtained by TEM, where the lateral correlation length was determined to be about
15&250nm and the screw dislocation density was of the order of 8 x lo8cmP2.
Further evidence that a small lateral correlation length causes Bragg peak broad-
ening is given in the reciprocal space map of figure 5. The reciprocal space map is
recorded by a series of S2-scans each having a slightly different detector position 2 0
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and the elliptical iso-intensity lines are shown. Peak broadening due to tilted growth
should lie parallel to the drawn S2-scan direction; peak broadening due to a small
lateral correlation length should lie parallel to the surface. The simultaneous pre-
sence of both effects results in an intermediate position of the ellipse. If, therefore,
only a S2-scan is performed on asymmetric reflections, the maximum broadening
cannot be measured. In principle, from the rotation angle with respect to the 52-
scan direction and the direction parallel to the surface, the values of the tilt angle and
the lateral correlation lengths can also be obtained (Fewster 1996), but because of
the small angle T (T is the tilt angle between surface normal and normal to the
diffracting plane; T # 0 for asymmetric reflections) this method was not used.
Figure 6 shows the @-scanof the asymmetric reflection 1015 of GaN. From this
broadening, a dislocation density of 1.2 x 10" cm-2 was obtained according to eqn.
( 5 ) for a random distribution of edge dislocations and a density of 2.3 x 10'' cm-2
was obtained according to eqn. (6) for small angle grain boundary formation, where

x
$-
- l.ox10-3
u)
v
-3
Sx10 -
11.5~10

-
1.0~10-~
-31 0, = O.9/(2Ll,) + a

X 1
z
2 5 . 0 ~ 16~-

0.0 0.1 0.2 Oi3 0.4 0.5 0.6 C ,7

(sin0)fi
Figure 4. Graphical separation of the lateral correlation length Lll and the tilt angle cyg using
the integral widths of the symmetric rocking curve. The straight line is a fit according to
the equation given in the plot.
 1022 T. Metzger et al.

0.006 -
GaN
1Oi4
-
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R Scan

4.006

-0.006 0.0 0.006

Aq I
Figure 5. Reciprocal space map to the 1014 reflection of GaN. The rotation of the intersect-
ing ellipse at half maximum intensity shows that both a lateral correlation length and a
tilted growth cause the observed Bragg peak broadening. The direction of the angular
scan (a-scan) is drawn as a line (qI1 and qL are reciprocal lattice units parallel and
normal to the substrate surface).

O -3
0.0 -2 m -1 0 2 1 2 m3
 Defects in epitaxial GaN51m.v 1023

Table 2. Measured and calculated-strain broadening of asymmetric reflections due to edge

dislocations with bE = f(1120) and screw dislocations with bs = [OOOl].
0, calculated deg
6
N~ = 1.0 x 10' cm1 2
Reflection 2 0 (deg) /, measured (deg)
3 Ns = 2.6 x lo* cm-2
1014 82.04 0.072 0.070
iois 104.99 0.094 0.087
ioi6 138.07 0.168 0.148
2024 109.15 0.144 0.182
2025 136.48 0.220 0.285

a lateral correlation length of 150nm was used as determined by TEM and XRD
measurements.
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For the determination of dislocation densities from the strain broadening of

asymmetric reflections, the resulting peak widths were calculated for different den-
sities of screw and edge dislocations using eqns. (8)-(12) and compared with the
measured widths. A correction for small correlation lengths was not necessary
because of the large correlation length normal to the substrate surface and the
relatively small angle T for the asymmetric reflections used (7 = Ys is the angle
between the diffracting plane normal and the substrate surface normal).
Asymmetric hh(2h)Z reflections can additionally be broadened by stacking faults
(Warren 1969, Fewster 1996). Therefore only h0hl-type reflections are used for the
determination of dislocation densities despite the fact that no stacking are observed
in the TEM measurements.
Table 2 shows the results for an edge dislocation density of 1 x 10'' cmP2 and a
screw dislocation density of 2.6 x lo8cmP2. The influence of the screw dislocation
density on the peak broadening is very small, until it reaches the order of the edge
dislocation density. This influence can, however, be neglected by considering TEM
measurements and the results obtained when using angles a@and a0 for determina-
tion of the dislocation density (eqns. (4) and (5)). Therefore, the simulated broad-
ening is very sensitive only to variations in the edge dislocation density.
From the values in table 2 it can be seen that, especially for higher diffraction
angles, the measured and calculated values of /?, differ from each other. Various
reasons for this can be proposed. Firstly, the present strain model is only valid for
isotropic systems and in general crystals are anisotropic media. Further, there is no
detailed information available regarding the acting range of the strain field of dis-
locations in GaN with its high binding energy, especially when values for ro are
unknown. Finally, the model does not consider the formation of small angle grain
boundaries, which lead to a decrease in the effective strain field acting around dis-
locations (Fewster 1989). Thus the edge dislocation density calculated by this model
is expected to be slightly lower than the real value.

5 4. CONCLUSIONS
By performing a combined TEM and XRD analysis on MOCVD grown a-GaN
on c-AI2O3,the structural parameters (correlation lengths parallel and normal to the
substrate surface, dislocation densities of screw and edge dislocations, heterogeneous
strain and tilt and twist angles of the individual crystallites) have been determined.
For the X-ray measurements two independent methods were used to determine the
edge dislocation density and both correlation lengths. Table 3 summarizes the results
 1024 T. Metzger et al.

Table 3. Summary of the structural parameters of the investigated GaN grown on c-plane
sapphire obtained by high resolution XRD and TEM.

Value Method
Lateral correlation length Lll 150-25Onm TEM
15Onm graphical method (Q-scans)
190nm pseudo-Voigt fit (Q-scan: eqn. (2 a))
Vertical correlation length LL l00Onm TEM (layer thickness)
1000nm Williamson-Hall plot
500 nm pseudo-Voigt fit (20-8-scan: eqn. (4a))
tilt angle an 0.13" graphical method (Q-scans)
0.10" pseudo-Voigt fit (&can: eqn. (2 b))
twist angle a* 1.3" @-scan
Edge dislocation density NE, Nk 1.0 x 10" cW2 TEM
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1.2 x 10" cm-2 a* (random distribution: eqn. (5))

Screw dislocation density Ns
Heterogeneous strain
parallel co: E~
2.3 x 1010cm-2 a* (piled up distribution: eqn. (6))
1.0 x 10'' cm-2 la, (strain broadening: eqns. (8Hl2))
4.4 x 10' cW2 eqn. (3) (an from graphical method
applied to 8-scans)
2.6 x 10' cm-2 eqn. (3) (an from pseudo-Voigt fit
applied to 8-scan)
3.7 1 0 - ~ Williamson-Hall plot
1.4 1 0 - ~ pseudo-Voigt fit (20-8-scani eqn. (4b))

obtained by the different methods for the investigated epitaxial films. Both comple-
mentary methods (XRD, TEM) are quite different in their method of obtaining
structural information, yet give results which are in good agreement.
Further investigations especially in the field of the substrate-layer interface
region with its high density of misfit dislocations will be performed. Furthermore,
a comparison of molecular beam epitaxy and MOCVD grown GaN with respect t o
typical structural defects and characterization of GaN/AlGaN heterostructures as
well as AlGaN films is intended.

ACKNOWLEDGEMENTS
This work was supported by the Deutsche Forschungsgemeinschaft (Stu 139/3)
and the Bayerische Kultusministerium (IX/2-52 C( 12)-61/27/87 107).

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