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High-temperature annealing of AlGaN: Stress, structural, and

compositional changes
S. Rajasingam, A. Sarua, M. Kuball, A. Cherodian, M. J. Miles et al.

Citation: J. Appl. Phys. 94, 6366 (2003); doi: 10.1063/1.1616639


View online: http://dx.doi.org/10.1063/1.1616639
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JOURNAL OF APPLIED PHYSICS VOLUME 94, NUMBER 10 15 NOVEMBER 2003

High-temperature annealing of AlGaN: Stress, structural,


and compositional changes
S. Rajasingam,a) A. Sarua, M. Kuball, A. Cherodian, and M. J. Miles
H. H. Wills Physics Laboratory, University of Bristol, Tyndall Avenue, Bristol BS8 1TL, United Kingdom
C. M. Younes
Interface Analysis Centre, Oldbury House, 121 St. Michael’s Hill, Bristol BS2 8BS, United Kingdom
B. Yavich and W. N. Wang
Department of Physics, University of Bath, Bath BA2 7AY, United Kingdom
N. Grandjean
Centre de Recherche sur l’Hétéroépitaxie et ses Applications, CRHEA-CNRS, Rue B. Grégory,
Sophia Antipolis, F-06560 Valbonne, France
共Received 13 December 2002; accepted 13 August 2003兲
The effect of high-temperature annealing on stress in Alx Ga1⫺x N in different ambients and at
different temperatures was studied using ultraviolet micro-Raman spectroscopy. Low (x⫽0.08) and
high (x⫽0.31 and x⫽0.34) composition AlGaN, grown by metalorganic chemical vapor deposition
共MOCVD兲 and molecular-beam epitaxy 共MBE兲, were compared. Compositional and morphological
changes were monitored using Auger electron spectroscopy 共AES兲 and atomic force microscopy
共AFM兲, respectively. The Raman results demonstrate that all samples exhibit maximum stress
changes in the compressive direction when annealed in an air ambient. AES confirms this to be due
to higher oxygen incorporation after annealing in the air ambient, and shows higher oxygen
incorporation in the vicinity of cracks and defects. MOCVD and MBE samples of a similar
composition were found to reach the same biaxial stress, despite differences in initial stress and
growth temperature. Relaxation of a parabolic intercrack stress profile to homogeneous stress was
observed with annealing in all ambients for cracked samples. AFM results on cracked samples show
an increase in width of the primary cracks along the 具 21̄1̄0 典 directions, and the formation of
secondary cracks along the 具 11̄00典 directions. © 2003 American Institute of Physics.
关DOI: 10.1063/1.1616639兴

I. INTRODUCTION perimental and theoretical studies of the local stress around


cracks in nitride layers have been reported by other
GaN, AlN, and Alx Ga1⫺x N are wide band-gap semicon- authors.5–7
ductors that have attracted great interest in recent years for High-temperature annealing is an important processing
high-power high-frequency device applications, due to their step in the fabrication of devices based on these materials.
high carrier mobility, high thermal conductivity, and high However, very little is known about the effects of annealing
breakdown field. Currently available substrates used for ep- on stress in AlGaN. Examples of the applications of anneal-
itaxial growth 共predominantly ␣ -Al2 O3 and 6H–SiC兲 have a ing include the activation of Mg acceptors and the fabrica-
poor lattice match and a large thermal expansion coefficient tion of ohmic contacts for these materials.8 In this work, we
mismatch to the III nitrides. This causes large stresses in the employ micro-Raman spectroscopy, atomic force microscopy
共AFM兲, and Auger electron spectroscopy 共AES兲 to monitor
grown epilayers. The crystalline quality often suffers in this
stress, morphology, and composition changes in AlGaN after
case, due to the introduction of cracks and defects into the
annealing in different ambients and at different temperatures.
material as stress relieving mechanisms. The study of stress
We also report on changes in the stress profile in the vicinity
and cracking phenomena is therefore of great interest for the of cracks in AlGaN, as a function of annealing ambient and
development of Alx Ga1⫺x N devices. Einfeldt et al.1,2 re- temperature. This is an extension of previous work per-
cently used spatially resolved cathodoluminescence 共CL兲 formed on high composition AlGaN (x⫽0.72) 共Ref. 9兲 to a
spectroscopy, X-ray diffraction and finite element modeling range of lower composition samples 共up to x⫽0.34).
to compare the biaxial strain profile in the vicinity of cracks
experimentally and theoretically. Romano et al.3 measured
the strain profile across a crack in a GaN layer and compared II. EXPERIMENTAL DETAILS
it to the elastic crack model of Atkinson et al.4 Similar ex- Three different samples were studied. Sample A is a 0.54
␮m thick Al0.34Ga0.66N layer on a 0.54 ␮m GaN layer de-
a兲
Author to whom correspondence should be addressed; electronic mail: posited on a sapphire 共0001兲 substrate by metalorganic
sr5026@bris.ac.uk chemical vapor deposition 共MOCVD兲. Sample B is a 1.2 ␮m

0021-8979/2003/94(10)/6366/6/$20.00 6366 © 2003 American Institute of Physics

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J. Appl. Phys., Vol. 94, No. 10, 15 November 2003 Rajasingam et al. 6367

thick Al0.31Ga0.69N layer on a 25 nm GaN buffer layer de-


posited on a sapphire 共0001兲 substrate by molecular-beam
epitaxy 共MBE兲. Sample C consists of a 1 ␮m thick
Al0.08Ga0.92N layer on a GaN nucleation layer deposited on a
sapphire 共0001兲 substrate by MOCVD. MOCVD samples
were grown at 1100 °C, whereas the MBE sample was grown
at approximately 830 °C. Sample A exhibits primary cracks
in the three equivalent 具 21̄1̄0 典 directions, whereas samples
B and C were uncracked, due to differences in composition
and growth conditions. This cracking behavior has been
shown to relax the tensile strain in the AlGaN layer.10 The
crack density 共inverse perpendicular crack spacing兲 is ap-
proximately 0.1 ␮m⫺1 for sample A, and is nearly uniform
over the sample surface.
The samples were annealed in a Linkham TS1500 an-
nealing stage at temperatures from 800 °C to 1200 °C for 15
min in air, oxygen, and nitrogen ambients. The E 2 phonon
mode was used to determine the stress in all samples, and
was measured in z(x,⫺)z̄ scattering geometry using a Ren-
ishaw micro-Raman system 2000 and the 325 nm line of a
He–Cd laser as the excitation source. In the case of cracked
samples, micro-Raman line scans were taken perpendicular
to primary cracks. AES was performed using a PHI micro-
probe 595 Perkin–Elmer system, upgraded with a field emis-
sion source. The beam conditions used were 3 keV, 15 nA,
and a 30° incident angle. The Auger transitions considered in FIG. 1. E 2 phonon frequency as a function of annealing temperature for
the measurement were Ga 共LMM, 1070 eV兲, Al 共KLL, 1396 annealing in 共a兲 air and 共b兲 nitrogen for samples A, B, and C. Also included
eV兲, N 共KLL, 381 eV兲, and O 共KLL, 510 eV兲. Relative com- is data for GaN 共from Ref. 12兲.
positions were derived by comparing the peak-to-peak am-
plitudes of the differentiated Auger spectra, corrected for the
appropriate elemental sensitivity factors.11 The elemental
sensitivity factors were checked using GaN, GaAs, and 1200 °C in a nitrogen ambient. Annealing in air at tempera-
Ti–Al–N samples of known compositions. Depth profiling tures up to decomposition causes the E 2 phonon frequency to
was achieved by Ar⫹ -ion sputtering, using an ion beam of increase with annealing temperature for all samples. Just
4 kV, 1.8 Am⫺2 at an incident angle of 60 °. The actual depth prior to decomposition, the phonon frequency approaches a
was estimated using TRIM software calculation. Morphology value for unstrained material, which manifests itself in Fig.
changes were measured by AFM, using a Digital Instruments 1共a兲 as a plateau in E 2 frequency for the higher composition
Dimension 3100 in tapping mode. samples, and a reduction in E 2 frequency for the lower com-
position samples. There is no significant change of E 2 pho-
non frequency with annealing in the nitrogen ambient for
III. RESULTS
samples B and C 关Fig. 1共b兲兴. Sample A uniquely shows a
Figure 1 summarises the stress changes with annealing small change of phonon frequency with annealing in nitro-
in air and nitrogen ambients for samples A, B, and C, to- gen, which will be discussed in more detail later.
gether with the results for the annealing of GaN from Hayes Stress relaxation near the cracks in sample A is evident
et al.12 The results for sample A correspond to measurements from spatial variations in the E 2 phonon frequency, as shown
taken away from the cracks, to minimize relaxation effects in Fig. 2. The inset of Fig. 2 is a reflected light image, with
from the cracks, allowing comparison to the uncracked the scanned region marked as a dotted line in Fig. 2. Similar
samples B and C. As-grown sample A has an E 2 frequency of stress profiles were recorded in different parts of the sample.
576.1 cm⫺1 共unstressed Al0.34Ga0.66N: 578.2 cm⫺1兲; as- The stress profile is approximately parabolic, as can be seen
grown sample B, 574.8 cm⫺1 共unstressed Al0.31Ga0.69N: from the thick full line in Fig. 2 fitted to the experimental
576.9 cm⫺1兲; and as-grown sample C, 570.3 cm⫺1 共un- results. Figures 3共a兲–3共c兲 show the results of micro-Raman
stressed Al0.08Ga0.92N: 569.4 cm⫺1兲. The relaxed E 2 phonon line scans across cracks in sample A under the various an-
frequencies are taken from Davydov et al.13 and were de- nealing conditions. A relaxation to a spatially homogeneous
rived from thick AlGaN layers. The higher composition phonon frequency is evident after annealing in all ambients,
samples are therefore under tensile stress as grown, whereas including nitrogen and oxygen. This phonon frequency cor-
the lower composition sample 共sample C兲 is compressively responds to tensile stress after nitrogen and oxygen ambient
stressed as grown. annealing, and relaxed stress after air ambient annealing.
During the high-temperature annealing, all samples start To identify the origin of the stress changes in the
to visibly decompose at approximately 1100 °C in air, and at samples, AES was performed on sample A to measure the

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6368 J. Appl. Phys., Vol. 94, No. 10, 15 November 2003 Rajasingam et al.

FIG. 2. E 2 phonon frequency of sample A as a function of position along the


surface. Inset is a reflected light image indicating the location of the line
scan. The thick line is a parabolic fit to the data. Crack locations are marked,
as is the reported unstrained phonon frequency for Al0.34Ga0.66N 共from
Ref. 13兲.

composition as a function of sample depth before and after


annealing in different ambients at 1000 °C. A thin surface
layer of residual hydrocarbons and other impurities was ini-
tially etched away before the measurements. The results are
shown in Fig. 4. The air-annealed sample shows significantly
greater oxidation than the samples annealed in other ambi-
ents. The nitrogen-annealed sample shows only a slightly
larger amount of surface oxygen as compared to the as-
grown sample. For the air-annealed sample, a map of the
oxygen signal was taken at a sample depth of approximately
300 nm 关Fig. 5共a兲兴. The highest oxygen signal is found to
correlate with the primary crack positions and local defects
关white arrows in Fig. 5共a兲兴. A map of the nitrogen signal
关Fig. 5共b兲兴 shows direct anticorrelation with the oxygen sig-
nal, suggesting that the oxygen replaces the nitrogen.
A high contrast AFM image of sample A after annealing
at 1000 °C in a nitrogen ambient is shown in Fig. 6共a兲. An
example of the formation of a crack is indicated by a line
arrow. These secondary cracks are formed in the 具 11̄00典 di-
rections, sometimes kinking in the 具 21̄1̄0 典 directions. The
inset of Fig. 6共a兲 shows high magnification AFM images of
other morphological surface features 共solid arrows兲. Hexago- FIG. 3. E 2 phonon frequency of sample A as a function of position between
nal pits of approximately 150 nm in diameter are present two cracks before and after annealing in 共a兲 air, 共b兲 nitrogen, and 共c兲 oxygen
both before and after annealing, possibly related to disloca- at various temperatures.
tions of screw or mixed type.14 Surface hillocks are formed
after annealing. They are approximately 20 nm in height and
of the order of 50–200 nm in diameter. They show no obvi- mation in these scans is not accurate, since the AFM tip is
ous symmetry, and can be understood by considering the not expected to penetrate fully into the cracks.
AES depth profile of the nitrogen-annealed sample A 关Fig.
4共b兲兴. The net loss of nitrogen and the small increase in the
IV. DISCUSSION
Al and Ga atomic fraction near the sample surface suggest
that these features are surface Ga droplets. The frequency of the E 2 Raman mode is linearly depen-
Figure 6共b兲 shows AFM height line profiles measured dent on stress, and is therefore a measure of the local stress
perpendicular to a primary crack before and after consecutive state of the samples. Higher phonon frequencies imply com-
annealing at 800 °C and 1000 °C in a nitrogen ambient. The pressive stress, whereas lower phonon frequencies imply ten-
approximate crack widths from this measurement are 30 nm sile stress 共as compared to the relaxed phonon frequency兲. As
as grown, 100 nm after 800 °C annealing, and 140 nm after a guide, one can assume a linear coefficient of 3 cm⫺1/GPa
1000 °C annealing. A definite crack widening is evident, independent of Al composition, based on currently reported
which is consistent with the decrease of tensile stress with data for AlN 共Refs. 15 and 16兲 and GaN,17,18 which quote
annealing, different from the behavior of uncracked samples values between 2.41 cm⫺1/GPa and 3.3 cm⫺1/GPa for GaN,
when annealed in nitrogen. Note that the crack depth infor- and between 2.55 cm⫺1/GPa and 4.4 cm⫺1/GPa for AlN.

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J. Appl. Phys., Vol. 94, No. 10, 15 November 2003 Rajasingam et al. 6369

FIG. 5. AES composition maps for sample A annealed in air at 1000 °C at a


depth of 300 nm, showing 共a兲 local oxygen concentrations and 共b兲 local
nitrogen concentrations. Local defects are marked with white arrows.

sample A, indicating that the stress changes discussed above


are related to the prescence of oxygen in the annealing
ambient.
The band gap of AlGaN at x⫽0.08 is smaller than the
UV excitation energy 共3.81 eV兲, so we expect the data for
sample B to be most sensitive to surface changes. This was
confirmed in measurements on sample B using a 2.54 eV
FIG. 4. Atomic fractions of Al, Ga, N, and O as a function of depth, derived excitation 共not shown in detail兲. These measurements, with
from AES measurements, for sample A 共a兲 as grown, 共b兲 annealed at
1000 °C in nitrogen, and 共c兲 annealed at 1000 °C in air. excitation energy below the band gap, show a behavior of the
E 2 phonon frequency similar to that shown in Fig. 1, but
with a maximum phonon frequency shift of only 2.5 cm⫺1
This is a necessary approximation since no deformation po- after annealing at 1000 °C in air. This is significantly smaller
tentials have been reported for the AlGaN alloy so far. than the 7.5 cm⫺1 shift observed under the UV excitation.
Figure 1 therefore illustrates the effect of annealing on This implies that the stress induced by annealing is mainly
stress in AlGaN for different compositions and different located near the sample surface.
growth methods. There is a repeatable maximum of com- Qualitatively, it can be seen from Fig. 2 that sample A is
pressive stress for annealing at a temperature of 1000 °C in under tensile stress as grown, which is approximately re-
an air ambient for the low composition sample (x⫽0.08). lieved in the vicinity of the cracks, although it must be noted
This maximum is attributed to the observed onset of sample that current literature values for the AlGaN E 2 phonon fre-
deterioration. This behavior is similar to that of GaN.12 The quency might not represent the fully relaxed state, and the
MBE sample C (x⫽0.31), although less tensile stressed as composition may not be accurately determined.13 Also note
grown, becomes relaxed to a similar level as the MOCVD that uniaxial stress components should be present in very
sample A (x⫽0.34) with annealing in air, despite the differ- close proximity to the cracks, but can be neglected here due
ent growth techniques and growth temperatures. The growth to the limited spatial resolution of the measurements 共⬃1
technique and the lower growth temperature of MBE there- ␮m兲. The experimental results are an average stress over the
fore do not significantly affect the stress state of AlGaN after depth of the AlGaN layer, since the electronic band gap of
annealing in air. Similar measurements performed after an- Al0.34Ga0.66N is 4 eV,19 which is higher energy than the 3.81
nealing in a nitrogen ambient show no significant changes in eV excitation, i.e., the laser fully penetrates the AlGaN layer.
stress for all samples 关Fig. 1共b兲兴, with the exception of The stress results show a parabolic stress profile 共thick full

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6370 J. Appl. Phys., Vol. 94, No. 10, 15 November 2003 Rajasingam et al.

This is confirmed here by AES measurements on sample


A. The air-annealed sample 关Fig. 4共c兲兴 shows oxygen to
completely replace the nitrogen to a depth of approximately
100 nm, and a significant presence of oxygen throughout the
sample. This is in contrast to the AES results for the
nitrogen-annealed sample 关Fig. 4共b兲兴. Since we analyze the
Raman modes of AlGaN, they must originate from a point
within the sample where the level of oxidation is sufficiently
low to have the vibrational properties of AlGaN, as opposed
to the properties of the oxides of Al or Ga at the top 100 nm
of the sample. Oxygen is preferentially incorporated in the
vicinity of the cracks and local defects, as seen in the Auger
map for sample A 共air annealed兲, etched to approximately
300 nm 共Fig. 5兲. This is not surprising, since cracked regions
and defects would allow oxygen to easily penetrate the
AlGaN layer. For uncracked samples, such as samples B and
C, oxygen incorporation would therefore more likely be con-
centrated at the vicinity of defects. The visible/UV Raman
results illustrate that these changes have the greatest effect
near the sample surface, as is expected from such an oxida-
tion process.
We note that stress changes also take place for sample A
when annealed in a nitrogen ambient 关Fig. 3共b兲兴. This is in
contrast to samples B and C 关Fig. 1共b兲兴, and is due to the
presence of cracks in this sample. Two stress relieving
mechanisms induced by annealing in a nitrogen ambient, that
are apparent from the AFM measurements, are the formation
of additional cracks and crack widening 关Figs. 6共a兲 and 6共b兲兴.
FIG. 6. AFM data for sample A. 共a兲 A high contrast height image after Additional possible mechanisms, from the results of Hearne
annealing in nitrogen at 1000 °C, with line and filled arrows marking a et al.,10 include the formation of misfit dislocations at the
secondary crack and a pit/hillock, respectively. Inset shows high magnifica-
tion AFM images of a pit and hillock. 共b兲 AFM primary crack depth profile AlGaN/GaN interface, which, aside from cracking, has been
before and after annealing in nitrogen at different temperatures. suggested as an alternative stress relieving mechanism in
these heterostructures.20 These stress changes might also
contribute to the observed stress changes when sample A is
line in Fig. 2兲 between the cracks of sample A. This is similar annealed in other ambients 共air and pure oxygen兲.
to recent stress measurements derived from CL measure-
ments of cracks in Al0.17Ga0.83N. 1 The change in the stress V. CONCLUSIONS
profile of sample A with annealing, as shown in Figs. 3共a兲–
3共c兲, shows two distinct effects. Annealing in a nitrogen or Ultraviolet micro-Raman measurements on stress in
oxygen ambient 关Figs. 3共b兲 and 3共c兲兴, shows a partial relax- Alx Ga1⫺x N layers show a stress change in the compressive
ation of the tensile stress between the cracks up to 1000 °C, direction for annealing in an air ambient up to 1000 °C for all
i.e., a stress change in the direction of compressive stress, compositions up to x⫽0.34. This appears as an increase in
finally resulting in a rather uniform tensile stress distribution compressive stress for the low composition sample (x
in the sample after annealing. Annealing in an air ambient ⫽0.08), and a reduction in tensile stress for higher compo-
共predominantly N2 , O2 , and H2 O) shows the same effect in sition samples (x⫽0.31 and 0.34兲. Higher composition
terms of uniformity of the stress profile, but shows higher samples (x⫽0.34 and x⫽0.31) grown by MOCVD and
stress change, in this case, resulting in an approximately MBE reach a similar stress state, despite differences in the
complete stress relaxation 关Fig. 2共a兲兴. This larger stress growth technique and initial stress state. AES and UV Raman
change for annealing in an air ambient as compared to an data on Al0.34Ga0.66N confirm these effects to be due to oxi-
oxygen ambient is in agreement with previous work showing dation in air, i.e., oxygen and the presence of water vapor,
the uniqueness of an air ambient on the high-temperature that occurs preferentially in the vicinity of defects and cracks
annealing of GaN,12 where a stress change in the compres- in the case of cracked samples. They also show the effects of
sive direction was found to be introduced by annealing in air. annealing in an air ambient to be most significant near the
This was speculated to be due to the incorporation of oxygen surface of the samples. Sample deterioration occurs at
into the layer by a process of wet oxidation, since no signifi- 1100 °C for annealing in an air ambient, and causes a relax-
cant stress change was found for annealing in a pure oxygen ation of stress in all the AlGaN layers. Sample deterioration
ambient. This is due to the presence of highly reactive OH⫺ occurs at 1200 °C for annealing in a nitrogen ambient. An-
radicals in annealing ambients containing water vapor, such nealing in a nitrogen ambient does not cause any significant
as air. change in the stress state of uncracked AlGaN. In cracked

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J. Appl. Phys., Vol. 94, No. 10, 15 November 2003 Rajasingam et al. 6371

7
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