Optical Materials 58 (2016) 491e496

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Optical Materials
journal homepage: www.elsevier.com/locate/optmat

Influence of crystallization front direction on the Mg-related impurity

centers incorporation in bulk GaN:Mg grown by HNPS method
B. Sadovyi a, b, *, M. Amilusik a, E. Litwin-Staszewska a, M. Bockowski a, I. Grzegory a,
S. Porowski a, M. Fijalkowski a, V. Rudyk b, V. Tsybulskyi b, M. Panasyuk b, I. Karbovnyk b,
V. Kapustianyk b
a
Institute of High Pressure Physics of the Polish Academy of Sciences, Sokolowska 29/37, 01-142 Warszawa, Poland
b
Ivan Franko National University of Lviv, Dragomanova 50, Lviv 79005, Ukraine

a r t i c l e i n f o a b s t r a c t

Article history: We studied the incorporation of Mg-related impurity centers in GaN crystals depending on the direction
Received 13 April 2016 of the crystallization front. Two series of GaN crystals e (i) undoped and (ii) Mg-doped e were grown by
Received in revised form High Nitrogen Pressure Solution (HNPS) method under otherwise identical conditions. Each series
1 June 2016
contained four samples with ð1010Þ, ð1120Þ, ð2021Þ and ð2021Þ orientations. The low-temperature
Accepted 16 June 2016
photoluminescence (PL) spectroscopy was used for characterization of the obtained crystals. The
Available online 30 June 2016
observed differences in the PL spectra of GaN:Mg crystals suggested that Mg incorporation in GaN grown
by HNPS method depends considerably on the orientation of crystallization front. The concentration of
Keywords:
Photoluminescence
Mg impurity incorporated into the GaN crystals subsequently increases for the following sequence of
Gallium nitride planes: ð1010Þ, ð1120Þ, ð2021Þ and ð2021Þ. For ð1010Þ, ð1120Þ and ð2021Þ planes the blue band is related
Mg impurity incorporation only to ON e MgGa donor-acceptor pair (DAP) transitions, while for ð2021Þ plane the incorporation of Mg-
Semi-polar orientation H complexes occurs additionally to the formation ON e MgGa DAP.
Non-polar orientation © 2016 Elsevier B.V. All rights reserved.
HNPS method

1. Introduction The incorporation of Mg in GaN was studied for layers grown

The discovery of the activation mechanism of p-type conductivity
in Mg-doped GaN (GaN:Mg) layers grown by Metal Organic Chemical
Vapor Deposition (MOCVD) method [1,2] has had a revolutionary
impact on the development of the technology of new generation
light sources [3] based on blue LED or blue/UV laser diodes. Mag-
nesium is still the only effective impurity that allows to obtain a p-
type conductivity in gallium nitride. This impurity also allows to
obtain the semi-insulating crystalline GaN substrates, being very
important for the creation of the High Electron Mobility Transistors
(HEMT) used in the high power high-frequency electronics [4].
Today, the market of the GaN-based devices is the second
biggest in the world, being the runner-up to the Si-electronics
market [5]. However, even though Mg is a crucial impurity for
light sources and transistors, the mechanisms of Mg incorporation
in GaN lattice are still insufficiently understood.
* Corresponding author. Institute of High Pressure Physics of the Polish Academy
of Sciences, Sokolowska 29/37, 01-142 Warszawa, Poland.
E-mail address: bsad@unipress.waw.pl (B. Sadovyi).
mainly by MOCVD and Molecular Beam Epitaxy (MBE) methods
with (0001) orientation. It was observed, that the concentration of
Mg incorporated in GaN grown by these methods significantly
depends on the concentration of the initial reagents [6e8] and the
growth temperature [6]. Still, the question about how Mg in-
corporates in GaN in case of specific directional growth remains
open. This question, however is of significant importance as the
experiments also indicated that changes of Mg concentration affect
optical properties [6,9,10] of GaN:Mg layers. Photoluminescence
spectra of GaN:Mg is shown to be strongly dependent on the
amount of Mg, but this effect has been mostly analyzed for epitaxial
layer grown on (0001) plane as summarized in Ref. [10].
Although some experiments on incorporation of Mg in GaN
layer on crystallographic planes other than (0001) were also per-
formed [11e14], there is still a lack of systematical knowledge about
the incorporation of Mg in GaN bulk crystals grown on different
crystallographic planes. It is also of particular interest in view of
already known [15e17] dependence of the concentration of incor-
porated oxygen in GaN on crystallization direction. In the present
work, we demonstrate that the mechanism of Mg incorporation can
be to some extent controlled at the stage of crystal growth by HNPS

http://dx.doi.org/10.1016/j.optmat.2016.06.027
0925-3467/© 2016 Elsevier B.V. All rights reserved.
492 B. Sadovyi et al. / Optical Materials 58 (2016) 491e496
method. For this purpose, we study low-temperature photo-
luminescence (PL) of a series of Mg-doped GaN single crystals
grown with different orientation of crystallization front using HNPS
technique [18]. For comparison, we also investigated the PL spectra
for a series of undoped GaN crystals grown by the same method at
the similar conditions. The variations in the PL spectra were
analyzed in order to draw correlations between the emission bands
and the Mg incorporation processes.
2. Materials and experimental methods
2.1. Investigated samples
GaN single crystals doped with Mg were grown by High Nitro-
gen Pressure Solution (HNPS) method [18] on GaN substrates sliced
from bulk GaN [16] crystallized by Halide Vapor Phase Epitaxy
(HVPE) [19]. The growth was performed for ð1010Þ, ð1120Þ, ð2021Þ
and ð2021Þ oriented substrates which were cut by diamond wire
saw in the form of rectangular stripes from free standing GaN HVPE
bulk crystals of 2 in. diameter and 5 mm thickness [16,17]. The
dimensions of the cut stripes were 20  5  0.4 mm. The growth
surfaces of all seed crystals were prepared before crystallization by
mechanical polishing by diamond powder and further chemical
mechanical polishing (CMP) procedure in the aqueous solutions of
KOH.
The crystallization was performed in a graphite crucible from
liquid gallium containing 0.5 at.% Mg at the following conditions:
1 GPa pressure of N2 gas, the growth temperature 1420  C and the
temperature gradient of about 30  C/cm, the time of growth e 50 h.
These conditions are typical for the growth processes by HNPS
method described in Ref. [18]. The series of undoped GaN single
crystals was grown for comparison at the same conditions, from
pure Ga.
After 50 h epitaxial growth, 20e30 mm thick GaN:Mg (GaN)
crystals were overgrown on top surfaces of the seeds. For optical
and other complementary measurements, 4  4 mm square sam-
ples were cut from the as-grown GaN and GaN:Mg crystals. The
geometry of a sample prepared for measurements is shown in Fig 1.
The surfaces for optical, X-ray diffraction (XRD) and Secondary
Ion Mass Spectroscopy (SIMS) measurements were prepared by
mechanical polishing by diamond powder. The damaged layer
induced by diamond was then removed by reactive ion etching
(RIE). Finally, the thickness of new GaN or GaN:Mg crystals on GaN
seeds were ca. 20 mm as indicated in Fig. 1.
Fig. 1. Typical geometry and dimensions (not to scale) of a GaN (GaN:Mg) sample
prepared for photoluminescence investigations. Laser beam is used as an excitation
source.
2.2. Experimental details of PL measurements
The PL spectra for all samples were measured at 11 K in a helium
atmosphere. A special optical cryostat equipped with a DE-202A
closed cycle cryocooler (Advanced Research Systems) was used to
cool down the samples. Stabilization of temperature was per-
formed by Cryocon 32 (Cryogenic Control Systems Inc.) tempera-
ture regulator. The emission was excited by FQSS266-Q2 laser
(CryLaS GmbH) operating at 266 nm with quasi-cw power of
14 mW. The lateral size of the laser spot was about 900 mm. The
profiles of the measured PL spectra do not depend on the excitation
intensity in this range. The luminescence spectra were measured
using automated spectrograph M266 (Solar LS) equipped with a
CCD-camera incorporating a Hamamatsu S7030-1006S sensor.
In order to check the possible inhomogeneity of the crystals, we
have measured spectra at three different points for each sample.
The PL spectra obtained for a particular sample were practically the
same, manifesting only slight intensity variations (less than 15%).
In order to analyze crystal quality, GaN:Mg samples were
studied by X-ray diffraction (XRD). The X-ray diffraction was carried
out using a high-resolution X-ray diffractometer Philips X’Pert Pro,
equipped with a four reflection Bartels monochromator and Cu Ka1
radiation source. The X-ray beam had dimensions of
3 mm  10 mm. The X-ray rocking curve scans (omega scans) were
measured with an open detector for the following reflections: (110)
for the ð1120Þ plane, (010) for the ð1010Þ plane and (201) for the
semi-polar planes.
Secondary ion mass spectroscopy (SIMS) method was used to
investigate magnesium, oxygen and hydrogen contaminations in
obtained crystals. SIMS measurements were performed for all
samples placed simultaneously in the measuring chamber.
3. Results
Assessment of crystal quality of grown crystals was performed
by measuring XRD omega scan rocking curves for respective re-
flections and determining full width at half maximum (FWHW) for
corresponding lines. Determined FWHM values are summarized in
Table 1.
From Table 1 data one can conclude that all obtained crystals are
of relatively high quality. Matching FWHM values of obtained GaN
crystals with values for GaN grown by the same technique on
(0001) plane [20] or with values for GaN grown by HVPE on non-
polar and semi-polar planes [16] we can see that the quality is
comparable. Comparative analysis of nominally undoped reference
GaN crystals and GaN:Mg crystals investigated in the present work
shows that adding Mg slightly decrease the crystal quality. Possible
reason is the formation of triangular inclusions (structural imper-
fections) that are known to appear during growth in HNPS-grown
GaN:Mg [18]. For both GaN and GaN:Mg we observe similar
trend: crystal quality of non-polar crystals is somewhat better than
that of the crystals, grown on semi-polar planes (as confirmed by
lower values of FWHM of rocking curves in case of non-polar
crystals).
In general, XRD data allow to say that crystal quality is high
enough to use these crystals for the studies of Mg incorporation in
GaN during the HNPS growth.
Prior to optical measurements, SIMS technique was employed to
determine the contamination of unintentional impurities (O and H)
in GaN and GaN:Mg crystals in order to account for their possible
influence on the PL spectra.
For GaN from the reference series it was established that prin-
cipal unintentional impurity is О, which is typical for HNPS growth
technique [18]. O concentration values in these crystals as
measured by SIMS are the following: 6.4  1019 cm3 (plane (10-
 B. Sadovyi et al. / Optical Materials 58 (2016) 491e496 493

Table 1
XRD results summary for all crystals grown in non-polar and semi-polar directions.

Crystal orientation Non-polar Semi-polar

ð1010Þ ð1120Þ ð2021Þ ð2021Þ

FWHM of rocking curves of GaN:Mg crystals, arcsec 228 265 314 305
FWHM of rocking curves of reference GaN crystals, arcsec 67 98 167 168

10)), 7.5  1019 cm3 (plane (11-20)), 2.4  1019 cm3 (plane (20-2-
1)) and 4.5  1019 cm3 (plane (20-21). Speaking of hydrogen, its
concentration is less than 3  1017 cm3, i.e. below the detection
limit.
SIMS data on GaN:Mg indicate that oxygen concentration is
comparable to that in unintentionally doped crystals. For crystals
grown on (10-10), (11-20) and (20-2-1) planes O concentration is
(3.2e3.8)  1019 cm3 and for crystal grown on (20-21) plane it
equals ca. 6.8  1019 cm3. Hydrogen concentration according to
SIMS data in GaN:Mg rises with respect to reference crystals and
equals 2  1018 cm3 for crystals grown on (10-10) and (20-21)
planes and 8  1018 cm3 for crystals grown on (11-20) and (20-2-
1) planes. However, using these data for unambiguous assessment
of incorporated hydrogen can be complicated due to considerable
error in determination of hydrogen concentration by SIMS tech-
nique. Therefore, further important conclusions about hydrogen
incorporation are made based on PL spectra analysis.
Thus, in this report we primarily focus on PL spectra measure-
ment, interpretation and analysis for GaN and GaN:Mg grown by
HNPS method. As already mentioned, the PL spectra of GaN:Mg
crystals with different orientations were measured with the refer-
ence to the PL spectra of the undoped GaN crystals with the same
orientations. The spectra for the two sets of investigated samples
are shown in Fig. 2. The PL spectra of the reference series of GaN
crystals (undoped) are presented in Fig. 2(a) and PL spectra of the
series of GaN crystals doped with Mg (GaN:Mg crystals) are
collected in Fig. 2(b).
As one can see from Fig. 2(a), all PL spectra of the reference
series of GaN crystals are quite similar and the emission within the
two spectral regions can be observed: near-band-edge (NBE) PL
peaked at 3.49 eV and yellow PL band (YB) with the maximum at
2.27e2.28 eV. The observed spectra are typical for unintentionally
oxygen doped GaN crystals grown by HNSP method [10,18]. A lower
intensity of NBE PL for GaN crystal grown on ð1120Þ plane in
comparison to other samples may be explained by a lower crys-
talline quality of this crystal.
The PL spectra of GaN:Mg crystals (see Fig. 2(b)) look qualita-
tively different from the reference spectra of GaN crystals due to the
considerable damping of NBE (3.48 eV) and YB (2.34e2.35 eV) PL as
well as because of the appearance of a new broad PL band in the
blue range of the spectrum (3.0e3.3 eV). The blue band (BB) is
interpreted as due to transitions between the energy levels corre-
sponding to the Mg impurity centers [6,10].
Both the shapes of the blue PL bands and their positions are not
identical for the samples with different orientations. For the sample
grown on the non-polar ð1010Þ plane, the BB PL is similar to the
typical band corresponding to donor-acceptor pair transitions with
LO-phonon replica [10,21]. The zero-phonon line (ZPL) has a
maximum at 3.28 eV and the two LO-phonon replica are positioned
at 3.19 and 3.10 eV. On the other hand, the crystals grown on the

Fig. 2. PL spectra measured at 11 K for: (a) the series of reference undoped GaN crystals, (b) the series of Mg-doped GaN crystals. For both series the red lines correspond to PL
spectra of crystals grown on ð1010Þ plane, the black lines e to the crystals grown on ð1120Þ plane, green and blue lines correspond to the crystals grown on a semi-polar ð2021Þ and
ð2021Þ planes, respectively. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)
494 B. Sadovyi et al. / Optical Materials 58 (2016) 491e496
non-polar ð1120Þ and semi-polar ð2021Þ planes exhibit only a
single broad blue luminescence band with a red shift of the peak to
3.12 and 3.11 eV, respectively. The broadest BB PL band with a larger
red shift to 3.02 eV was observed for sample grown on the semi-
polar ð2021Þ plane. The large shape asymmetry of the low-energy
side of BB PL is connected with appearance of an additional PL
band peaked around 2.7e2.9 eV and overlapping with the band
centered around 3.02 eV.
Decrease of NBE and YB PL intensities in comparison with those
in the undoped GaN crystals is typical for GaN:Mg crystals grown
by HNSP method [22] and other techniques [7,23]. The strong
decrease of the YB intensity for GaN:Mg is due to reduction of
gallium vacancies (VGa) concentration [24] responsible for the yel-
low luminescence [25e27] in GaN. Smearing of the NBE lumines-
cence peak is likely due to increasing number of excitons localized
on the acceptor impurity [10].
The data on the band positions in the measured PL spectra are
summarized in Table 2. The analysis and comparison of the ob-
tained PL spectra in respect to the results of the previous studies are
included into the next section below.
4. Discussion
The observed changes of the band shapes and the redshift of BB
PL peak from 3.28 to 3.02 eV depending on the orientation
(Fig. 2(b)) were found to be very similar to the changes observed
previously for BB PL of (0001) oriented GaN:Mg layers due to the
increase of Mg concentration from 2  1019 cm3 to 8  1019 cm3
[6]. It is important to notice that in GaN:Mg layers grown by
MOCVD [6,10] or MBE [10,21] on (0001) plane the concentration of
Mg was increased intentionally. For these layers the luminescence
was usually related to DAP transitions [6,10,21], where the shallow
donor was probably a nitrogen vacancy (VN) and the shallow
acceptor was MgGa (see the scheme in Fig. 3(a)) [10]. The changes of
BB PL in GaN:Mg crystals grown in different directions in this work
are very similar to those observed by the authors of [6] for GaN:Mg
layers with different Mg impurity concentrations grown in [0001]
directions. Therefore, we suggest that in the case of GaN:Mg crys-
tals grown by HNPS method the observed changes of BB PL are
related to different concentration of incorporated Mg in GaN
crystals grown on different planes in spite of the fact that the
growth was performed under identical conditions. This allows to
conclude that the mechanism of Mg impurity incorporation varies
for different directions of crystallization front.
As it follows from Fig. 2(b), the lowest amount of Mg should be
incorporated into GaN:Mg crystal grown on ð1010Þ plane whereas
the highest one e into the crystal grown on ð2021Þ plane. These
expectations were supported by the Secondary Ion Mass Spec-
troscopy data concerning Mg concentration for these planes: the
lowest measured concentration was found to be 2  1019 cm3 and
Table 2
Energy of peaks in PL spectra of GaN and GaN:Mg single crystals grown at different orientations of the crystallization front by HNPS method.
Crystal orientation PL yellow band, eV
GaN:Mg crystals
Non-polar ð1010Þ plane 2.35
Non-polar ð1120Þ plane 2.35
Semi-polar ð2021Þ plane 2.34
Semi-polar ð2021Þ plane e 3.02
Reference GaN crystals
Non-polar ð1010Þ plane 2.29
Non-polar ð1120Þ plane 2.27
Semi-polar ð2021Þ plane 2.29
Semi-polar ð2021Þ plane 2.29
Fig. 3. Scheme of the radiative transitions between the impurity related donor and
acceptor levels within GaN energy gap: (a) GaN:Mg MOCVD or MBE layers; (b) GaN:Mg
single crystals grown by HNPS method.
the highest e ca. 6  1019 cm3 for ð1010Þ and ð2021Þ growth
planes, respectively.
Taking into account that BB PL is due to DAP transitions it should
be noted that in the crystals grown by HNPS the dominating
shallow donor is oxygen [22,28], in contrast to MOCVD grown
GaN:Mg, where the shallow donor is usually VN [29]. This is the
consequence of the fact that ON incorporation is energetically more
favorable than that of VN [30] and that the HNPS growth system is
strongly contaminated with oxygen. The energies of ON [31] and VN
[29] levels are of about 30e40 meV below the conduction band.
Therefore, for the GaN:Mg crystals grown by HNPS method, ON
plays the same role as VN does in the GaN:Mg layers grown by
MOCVD or MBE. Consequently, the BB of PL spectra for both cases
are identical due to the similar number of the donor-acceptor pairs
(see the scheme in Fig. 3(b)).
The band at 3.02 eV in the spectrum of GaN:Mg grown on ð2021Þ
plane is asymmetric in a high degree. This indicates that not only
DAP transitions are responsible for the formation of the band. It is
well-known that for p-type GaN:Mg layers the band at
2.75e2.85 eV [2,10,32,33] with peak position weakly dependent on
the Mg concentration appears in the PL spectra [8,34]. This band
was also observed in the H-passivated GaN:Mg crystals that can be
activated to exhibit a p-type conductivity [9,35,36]. Thus, it is
plausible to assume that this band can also be present in the
measured spectrum of GaN:Mg grown on ð2021Þ. This assumption
is confirmed by a Gaussian decomposition of the complex band
depicted in Fig. 4 into three peaks centered at 2.35, 2.85 and
3.05 eV. The components peaked at 2.35 eV and 3.05 eV were also
observed in the spectra of other crystals from the Mg-doped series
(Fig. 2(b)). These components are YB PL and BB PL related to DAP
transitions, respectively. The band at 2.85 eV results from the op-
tical transitions due to the transformation of Mg impurity from the
state with a strongly localized hole to the neutral charge state [37].
PL blue band, eV PL near-band-edge line, eV
3.28/3.19/3.10 3.47
(ZPL/1LO/2LO)
3.12 3.47
3.11 3.48
3.48
e 3.50
e 3.50
e 3.50
e 3.50
 B. Sadovyi et al. / Optical Materials 58 (2016) 491e496
Fig. 4. Gaussian decomposition of the broad blue-yellow PL band of GaN:Mg crystal
grown on ð2021Þ plane. (For interpretation of the references to colour in this figure
legend, the reader is referred to the web version of this article.)
Appearance of the band at 2.85 eV can be considered as an evidence
that Mg-H complexes are incorporated into the lattice of the GaN
crystal grown on ð2021Þ plane.
Recent experiments have shown a full compensation between
Mg related shallow acceptors and ON shallow donors [38] in semi-
insulating GaN:Mg crystals grown by HNPS method on (0001)
plane. Accordingly, their PL spectra in blue region had only bands
related to DAP transitions. These PL spectra are similar to those
which are measured in the present work for GaN:Mg crystals
grown on ð1120Þ and ð2021Þ planes. Therefore in GaN:Mg crystals
with ð1120Þ and ð2021Þ orientations the full compensation of MgGa
acceptor by ON donors (the same concentrations of donor and
acceptor impurities) is very probable and we can assume that these
crystals are semi-insulating. In contrast, for GaN:Mg crystals grown
in ð2021Þ direction, our studies show that full compensation be-
tween donors and acceptors does not occur. This fact can be
explained by less effective incorporation of oxygen during growth
on this plane and two competition processes: incorporation of
isolated ON donor e MgGa acceptor pairs, which are mutually
compensated and incorporation of MgGa creating electroneutral
complexes with H.
The incorporation of Mg-H complexes in the GaN:Mg crystal-
lized spontaneously by HNPS method growing mostly in semi-
polar directions was suggested earlier [38], where the authors
report 50 meV redshift for BB PL peak of those GaN:Mg crystals
after annealing. The suggested Mg-H complexes dissociated after
the annealing and concentration of the non-compensated Mg im-
purity raised as it was confirmed by detection of p-type conduc-
tivity in these crystals [38]. Our studies suggest that the
incorporation of Mg-H complexes is observed only for growth on
ð2021Þ plane and consequently only these crystals can have a p-
type conductivity after annealing. Although in the present work the
GaN:Mg crystals with ð2021Þ orientation were not annealed, a
certain amount of non-compensated Mg impurity is present any-
way, enabling the optical transitions, responsible for 2.85 eV band.
Increasing of 2.85 eV band intensity and detection of p-type con-
ductivity is therefore, expected after annealing.
5. Conclusions
Based on the analysis of the low-temperature PL spectra it is
shown that mechanisms of Mg impurity incorporation into the GaN
crystals during their growth by HNPS method are different for
495
various crystallographic orientations. In particular, concentration of
incorporated Mg depends on the direction of crystallization front.
It is determined that the influence of crystallization front di-
rection is most notable for ð2021Þ plane. We suggest that during
growth on this plane there exist two well-pronounced concurrent
processes: incorporation of Mg-H complexes and simultaneously
the incorporation of Mg and O impurities forming the donor-
acceptor pairs. For the other orientations under study, the incor-
poration of donor-acceptor pairs is dominant. This allows to assume
that the crystals grown on ð2021Þ plane should have a p-type
conductivity after activation of Mg-acceptor in contrast to those,
grown on ð1120Þ and ð2021Þ, which should be semi-insulating.
Acknowledgments
The research leading to these results has received financial
support from National Science Center Poland grant no. UMO-2012/
05/N/ST3/02545.
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