Journal of
Materials Chemistry C
COMMUNICATION
High internal quantum efficiency ZnO/ZnMgO
multiple quantum wells prepared on GaN/sapphire
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Cite this: J. Mater. Chem. C, 2019,
7, 6534 templates for ultraviolet light emitting diodes†
Received 15th March 2019,
Accepted 17th May 2019 Shanshan Chen,‡a Chenxiao Xu,‡b Xinhua Pan,
Jingyun Huang, b Bin Lub and Zhizhen Ye*b
DOI: 10.1039/c9tc01421g
rsc.li/materials-c
5-Period ZnO/Zn0.9Mg0.1O Multiple Quantum Wells (MQWs) were
fabricated by plasma-assisted molecular beam epitaxy. The dominant
edge threading dislocations in epitaxial films were dramatically
reduced by using GaN/Al2O3 as substrates. As a result, a record high
internal quantum efficiency of 61% at 300 K was obtained for the
ZnO/Zn0.9Mg0.1O MQWs.
ZnO has attracted renewed attention due to its potential use in
high-efficiency ultraviolet light emitting diode (LED) and laser
diode (LD) devices due to its natural wide band gap of 3.37 eV
and large exciton energy of 60 meV, along with the benefits of
it being cheap, nontoxic and environmentally friendly.1–3
Besides n-type and p-type conduction in ZnO, the realization
of high efficiency multiple quantum wells (MQWs) is also an
important part in fabricating modern light emitting devices.
In this context, ZnO/ZnMgO MQWs are of particular interest
because they are free of toxic substances like Be and Cd.4 The
structural and optical properties of ZnO/ZnMgO MQWs have
been widely demonstrated by several groups.5–8 Electrically
pumped light emission and lasing actions in ZnO/ZnMgO
MQWs have been observed in ZnO homojunction light emit-
ting devices.9–12 However, there are still several challenges in
achieving high-efficiency ZnO based light emitting devices.
One of the major problems is that the internal quantum
efficiency (IQE) of ZnO/ZnMgO MQWs is so low. As is known,
IQE is one of the most important parameters to judge the
quality of a light emitting material. The best IQE value for
ZnO/ZnMgO MQWs is only 30%.13 Finally, their low IQE would
seriously restrict the performance improvement of LED or LD
a
School of Materials and Energy, Guangdong University of Technology,
Guangzhou 510006, People’s Republic of China
b
State Key Laboratory of Silicon Materials, Cyrus Tang Center for Sensor Materials
and Applications, School of Materials Science and Engineering,
Zhejiang University, Hangzhou 310027, People’s Republic of China.
E-mail: panxinhua@zju.edu.cn, yezz@zju.edu.cn
† Electronic supplementary information (ESI) available. See DOI: 10.1039/c9tc01421g
‡ These authors contributed equally.
6534 | J. Mater. Chem. C, 2019, 7, 6534--6538
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*b Haiping He, b
devices. It is highly desirable to improve the IQE of ZnO/
ZnMgO MQWs.
Defects and threading dislocations (TDs) which act as non-
radiation centers are detrimental to the IQE.14 It is known that
improving the crystalline quality of GaN films on free-standing
GaN substrates would decrease the non-radiative recombina-
tion between the defects and carriers, and thus increase the
IQE.15,16 And the improvement of crystalline quality is one of the
key factors in solving the problems associated with efficiency
droop in high-operating-current LED devices.17,18 On the basis of
these research studies, it is suggested that the higher crystalline
quality of epitaxial films results in a higher IQE.
As for the epitaxial growth of ZnO films and ZnO/ZnMgO
MQWs, sapphire and Si are the very popular commercial
substrates at present. However, the lattice mismatch between
sapphire and ZnO is still as high as 18.4% even after the optimized
epitaxial process with the 301 in-plane rotation, while the lattice
mismatch between Si and ZnO is even higher.3 The large lattice
mismatch leads to a high density of dislocations in epitaxial
films and structures, which reduces the mobility and shortens
the lifetime of carriers, and eventually deteriorates the IQE. In
addition, nearly lattice-matched ScAlMgO4 (SCAM) is also used
as a substrate for the growth of ZnO/ZnMgO MQWs. However,
the related research is limited for the reason that SCAM sub-
strates are less available and very expensive.19 As for homoepi-
taxial ZnO/ZnMgO MQWs, the highest IQE is only 20%.20 The
improvement is strongly dependent on the growth of large size
single crystal ZnO.
Considering the issues of the substrates mentioned above,
GaN seems to be a suitable substrate for the epitaxial growth of
high quality ZnO/ZnMgO MQWs, because GaN has the same
crystalline structure as and a closely matched lattice with a lattice
mismatch of 1.8% to ZnO.4 And high quality GaN/sapphire
templates are commercially available. Therefore, in this work,
GaN/sapphire is used as the substrate to fabricate high quality
ZnO/ZnMgO MQWs. The crystalline qualities of ZnO and ZnMgO
layers are investigated, and a record high IQE at 300 K of 61% for
This journal is © The Royal Society of Chemistry 2019

Communication
ZnO/ZnMgO MQWs is demonstrated. Then, the ZnO/ZnMgO
MQWs are used as an active layer to fabricate light emitting
devices, and electrically pumped ultraviolet light emission from
the MQWs is observed. A record high IQE at 300 K of 61% is
obtained in the ZnO/Zn0.9Mg0.1O MQWs. The greatly enhanced
IQE will give a boost for ZnO to the applications in high-
efficiency light emitting devices.
ZnO/ZnMgO MQWs were grown on commercially available
p-GaN/Al2O3 templates via the plasma-assisted molecular beam
epitaxy (MBE) technique. A thin low-temperature ZnO layer was
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deposited as a buffer layer. 5-Period ZnO/ZnMgO MQWs were
subsequently grown on the buffer layer at 650 1C. Elemental
zinc (6N grade), magnesium (6N grade) and oxygen radio-
frequency plasma (O2 gas, 6N grade) were used as the sources.
The Zn cell temperature, Mg cell temperature, oxygen flow rate
and radio frequency excitation power were fixed at 250 1C,
350 1C, 1.0 sccm and 300 W, respectively. The thicknesses of the
ZnMgO barrier layer and the ZnO well layer were 10 nm and
2 nm, respectively. For comparison, ZnO/ZnMgO MQWs were
also prepared on sapphire substrates. For the fabrication of a
light emitting diode, a low-temperature ZnO buffer layer, a
10 nm thick Zn1 xMgxO layer, 5-period ZnO/ZnMgO MQWs and
an undoped ZnO layer were deposited on a GaN/Al2O3 template
in sequence. The top layer of the GaN/Al2O3 template was 2 mm
Mg doped GaN. The electrical properties of the Mg doped GaN
layer were investigated by the van der Pauw method with Hall
measurements, and it showed p-type conduction with a hole
concentration of 5.30  1017 cm 3 and a Hall mobility of
14.7 cm2 V 1 s 1. Thus, the Mg doped GaN and undoped ZnO
layers were used as p-type and n-type layers, respectively. Bilayer
Ni/Au and Sn electrodes were used as the contacts for the p-GaN
and n-ZnO layers, respectively.
In order to investigate the crystalline quality, single-layer
ZnO and ZnMgO films were grown under the same growth
conditions. High-resolution X-ray diffraction (XRD) was used to
characterize the crystalline quality of the single-layer films. The
Mg content of the ZnMgO film was determined to be 10% by
X-ray photoelectron spectroscopy (XPS). Henceforth, the Mg
content in the ZnMgO barrier layer was determined to be 10%.
Photoluminescence (PL) measurements were used to analyze
the optical properties of the MQWs, which employed a 25 mW
He–Cd laser operating at a wavelength of 325 nm as an
excitation source and performed on an FLS920 (Edinburgh
Instruments) fluorescence spectrometer. Electroluminescence
(EL) measurements were carried out using a PL instrument, and
a continuous-current power source was used to excite the diode.
X-ray rocking curves will be broadened as the planes are
distorted by TDs.21 Thus, the crystalline quality of the epitaxial
films can be characterized by high-resolution XRD. Generally,
the full width at half maximum (FWHM) value of the on-axis
o scan is related to screw TDs, while that of the off-axis o scan
is responsible for edge TDs.21,22 A complete description of the
TDs requires both out-of-plane and in-plane distortions to be
fully specified. Here, both the surface normal (002) plane and
the off-axis (102) plane have been examined. Fig. 1 shows the
XRD o-rocking curves of the ZnO (002) and (102) diffraction
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Journal of Materials Chemistry C
Fig. 1 XRD o-rocking curves of (a) (002) and (b) (102) diffraction peaks
for ZnO and Zn0.9Mg0.1O layers grown on GaN/Al2O3 substrates. XRD
o-rocking curves of (c) (002) and (d) (102) diffraction peaks for ZnO and
Zn0.9Mg0.1O layers grown on Al2O3 substrates. The solid lines are pseudo-
Voigt fittings of the rocking curves.
peaks for single-layer ZnO and Zn0.9Mg0.1O films grown on
GaN/Al2O3 templates. The FWHM values of the (002) o-rocking
curves are 218 and 223 arcsec for the ZnO film and the
Zn0.9Mg0.1O film, respectively. As for the (102) rocking curves,
there are two recognizable diffraction peaks. For the reason
that GaN has very similar lattice constants to ZnO, both GaN
(102) and ZnO or Zn0.9Mg0.1O (102) diffraction peaks are
detected. Based on the fact that the FWHM value of single-
layer GaN (102) is 303 arcsec (Fig. S1, ESI†), the narrower one of
about 300 arcsec is confirmed as the GaN (102) diffraction peak
and the broader one is confirmed as the ZnO or Zn0.9Mg0.1O
(102) diffraction peak. Therefore, the FWHM values of the (102)
rocking curves are 667 and 681 arcsec for the ZnO film and the
Zn0.9Mg0.1O film, respectively. The relatively large FWHM
values of off-axis diffraction scans indicate that edge TDs are
dominant in the epitaxial ZnO and Zn0.9Mg0.1O films, which is
the common result in epitaxial ZnO and GaN films.22,23 For
comparison, the rocking curves of ZnO and Zn0.9Mg0.1O films
prepared on sapphire substrates are also investigated, as shown
in Fig. 1(c) and (d). The FWHM values are shown in Table S1
(see the ESI†). Compared with the films grown on the GaN/Al2O3
templates, the films grown on sapphire show narrower (002)
rocking curves and broader (102) rocking curves, which indicates
that screw TDs are really fewer in the films grown on sapphire
and edge TD densities are still high. Despite the fact that screw
TDs are more in the films grown on the GaN/Al2O3 templates,
the dominant edge TDs are significantly reduced. The relatively
small FWHM values of the (102) rocking curves indicate low
total defect densities in the epitaxial films fabricated on the
GaN/Al2O3 templates.
High quality single layer ZnO and Zn0.9Mg0.1O have been
confirmed. The optical properties of the 5-period ZnO/Zn0.9Mg0.1O
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Journal of Materials Chemistry C
Fig. 2 (a) PL spectrum at 80 K of ZnO/Zn0.9Mg0.1O MQWs grown on a
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GaN/Al2O3 substrate. The inset shows the integrated PL intensity of the LE
emission for the MQWs as a function of temperature. (b) PL spectra at 300 K
and 15 K of the ZnO/Zn0.9Mg0.1O MQWs grown on a sapphire substrate.
MQWs have been investigated. Fig. 2(a) shows the PL spectrum of
the MQWs at 80 K. There are two peaks located at 3.435 eV and
3.021 eV, respectively. The dominant peak at 3.435 eV is attributed
to the recombination of localized excitons (LEs) in the MQWs. It is
noteworthy that only the LE emission is observed in the higher
energy area and emissions from the Zn0.9Mg0.1O barriers are not
apparent. This indicates that carriers are confined efficiently in
the well regions. The weak peak at 3.021 eV is attributed to the Mg
doped GaN layer.24 The MQWs are so thin that emissions from the
Mg doped GaN layer underneath can be detected. The PL
spectrum is well consistent with the structure. As for determining
the IQE, an equivalent IQE of the LE emission peak at 300 K
deduced by PL measurement is used instead since the direct
measurement is very complicated. The IQE at 300 K is approxi-
mated as the integrated PL intensity at 300 K divided by that at
low temperature below when the emission shows a plateau. This
optical method is described in detail by Kawakami,25 and has
been widely applied.26–30 The measurement is explained in detail
in the ESI.† The inset in Fig. 2 shows the integrated PL intensity of
the LE emission for the MQWs grown on GaN/Al2O3 templates as a
function of temperature. The intensity changes a little when the
temperature is below 50 K. Therefore, the IQE is derived as the ratio
of the emission intensity at 300 K to that at a low temperature
below 50 K. Finally, the MQWs show a markedly high IQE of 61%.
The internal quantum efficiency of the emission can also be written
in terms of trad and tnon-rad: IQE = tnon-rad/(trad + tnon-rad); where trad
and tnon-rad denote the radiative and non-radiative lifetimes.
Accordingly, there is a positive correlation between the non-
radiative lifetime and IQE. Thus, the elimination of the non-
radiative lifetime is eagerly anticipated. And the edge TDs are the
dominant non-radiative recombination centers in epitaxial ZnO
films.14,22 As previously investigated, the edge TDs have been
dramatically reduced by using GaN/Al2O3 templates as sub-
strates, which has been confirmed by the relatively small FWHM
values of the off-axis XRD diffraction scans. Therefore, a high
IQE with low edge threading dislocations has been achieved by
using GaN/sapphire as the substrates. By contrast, the IQE of
MQWs deposited on sapphire is dramatically decreased. The PL
spectra at 300 K and 15 K of the MQWs grown on sapphire are
exhibited in Fig. 2(b). Two types of excitonic emission from the
ZnO wells at 15 K can be distinguished on a logarithmic scale,
which are denoted as the LE band and free exciton (FE) band,
6536 | J. Mater. Chem. C, 2019, 7, 6534--6538
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respectively. The integrated PL intensity of the excitonic emis-
sion at 300 K divided by that at 15 K is about 23%. It is thus
evident that the poorer crystalline quality with more edge TDs is
one of the significant factors in severely reducing the IQE.
Fig. 3 shows a review of the reported IQEs for ZnO/ZnMgO
MQWs, ZnO films and nanostructures (the details are shown in
Table S2, ESI†).13,19,20,27–34 The MQWs with the highest IQE of
30% were grown on c-plane sapphire.13 It is worth mentioning
that the IQE of MQWs is commonly higher than that of ZnO
films. The highest IQE is only 9.6% for the ZnO film, which was
epitaxially grown on a Zn-polar ZnO substrate.27 This indicates
that ZnO/Zn0.9Mg0.1O MQWs can realize high luminescence
efficiency. The nanostructures are supposed to have a higher
emission efficiency due to the fewer defects and excitons bound
to surface defect states. The best IQE of 33% was achieved for
ZnO nanorods grown on a 6H-SiC substrate.31 Compared to
these values, an IQE of 61% in this work is a remarkable record.
This reveals that using GaN/Al2O3 templates for the epitaxial
growth of ZnO/Zn0.9Mg0.1O MQWs is an efficient way to reduce
TDs, which is significant for the enhancement in light emission
IQE. The significantly enhanced crystalline quality and greatly
increased electron–hole recombination rate in the ZnO/Zn0.9Mg0.1O
MQWs grown on GaN/Al2O3 templates will finally improve the
performance of light emitting devices.
The I–V characteristics of a GaN/(ZnO/Zn0.9Mg0.1O MQWs)/n-
ZnO diode are shown in Fig. 4(a). It exhibits good rectification
with a turn-on voltage of about 3 V. Both the Sn electrodes in
contact with the n-type ZnO layer and the bilayer Ni/Au electro-
des in contact with the p-type GaN layer show good ohmic
behavior, as shown in the inset of Fig. 4(a). The ohmic contact
confirms that the rectification arises from the p–n junction.
Fig. 4(b) shows the EL spectrum of the diode operated under
forward current. A dominant narrow UV emission and a weak
deep-level emission are observed. For the purpose of better
understanding the EL results, the PL emissions from the p-GaN
layer and ZnO/Zn0.9Mg0.1O MQWs at room temperature are
taken as references, as shown in Fig. 4. The emission peaks of
the p-GaN layer and MQWs are located at 435 nm and 366 nm,
respectively. Obviously, the UV emission in the EL spectrum of
the diode is not derived from the p-GaN layer. It originates from
the LE recombination in the MQW active layer, which is desir-
able for LED and LD applications. There is a common issue for
Fig. 3 A summary of the reported IQEs for ZnO/ZnMgO MQWs, ZnO films
and nanostructures. The IQE reported in this work has been highlighted with
a red star.
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Communication
Fig. 4 (a) I–V curve of a p-GaN/(ZnO/Zn0.9Mg0.1O MQWs)/n-ZnO diode.
The inset shows the I–V curves of the Ni/Au electrodes on the GaN layer
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and the Sn electrodes on the ZnO layer. (b) EL spectrum of the GaN/(ZnO/
Zn0.9Mg0.1O MQWs)/n-ZnO diode, with the addition of normalized PL
spectra of p-GaN and MQWs at room temperature.
p-GaN/n-ZnO LEDs that carrier-recombination is often in the
p-GaN layer due to the easy drift of electrons into p-GaN.35 In
this work, carriers are confined in high-quality MQW well layers
and efficient carrier-recombination in MQWs is realized.
In summary, high quality ZnO and Zn0.9Mg0.1O layers have
been grown on GaN/Al2O3 templates. The FWHM values of the
(102) XRD rocking curves are only 667 and 681 arcsec for the
ZnO film and the Zn0.9Mg0.1O film, respectively. The related
dominant edge TDs have been dramatically reduced by using
GaN/Al2O3 substrates. With the reduction of TDs, the IQE of the
ZnO/Zn0.9Mg0.1O MQWs fabricated on the GaN/Al2O3 substrate
is significantly improved, and a record high IQE at 300 K of
61% is achieved. Electrically pumped light emission in the
ZnO/Zn0.9Mg0.1O MQWs has been observed. The excellent light
emitting properties of the ZnO/Zn0.9Mg0.1O MQWs are very
promising for high-efficiency ZnO-based light emitting devices.
Conflicts of interest
There are no conflicts to declare.
Acknowledgements
This work was supported by the National Natural Science
Foundation of China under Grant No. 91833301, the Zhejiang
Provincial Natural Science Foundation of China under Grant
No. LY17E020005, and the Fundamental Research Funds for
the Central Universities under Grant No. 2019FZA4006.
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