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Diamond in Tellurite Glass: a New Medium for Quantum
Information
M. R. Henderson,* B. C. Gibson, H. Ebendorff-Heidepriem, K. Kuan, S. Afshar V.,
J. O. Orwa, I. Aharonovich, S. Tomljenovic-Hanic, A. D. Greentree, S. Prawer,
and T. M. Monro
Quantum mechanics has defined twentieth century technology
and quantum information science has been identified as poten-
tially one of the most disruptive technologies of the twenty-
first century.[1] A major challenge for the development of this
field is the requirement to create a quantum-classical inter-
face to efficiently allow quantum information to be integrated
with a photonic backbone. As such, componentry needs to be
developed that places quantum emitters in the bound modes
of photonic structures. In recent years, diamond color centers
have become one of the most important platforms to exhibit
room-temperature quantum effects.[2] Here we demonstrate a
new medium suitable for quantum information consisting of
diamond nanocrystals embedded in a tellurite glass, and have
taken this material through an optical fiber drawing process.
Single photon emission was demonstrated from the drawn
material. By including diamond color centers within a soft
glass we open the possibility of leveraging all of the designs of
microstructured optical fibers[3] and optical cavities to integrate
quantum emitters with bound optical modes.
Tellurite is a promising base material for photonic structures
that has until now been overlooked for diamond applications.
It has a wide transparency window, from 500 nm to 4 μm, and
low transmission loss at the emission wavelengths of diamond
color centers (∼1 dB m−1 from 550–900 nm).[4] The high refrac-
tive index of tellurite (n ≈ 2 at 700 nm) allows the possibility
of forming high-Q cavity structures, and a high non-linear
refractive index and photosensitivity both permit the tuning of
M. R. Henderson, Dr. H. Ebendorff-Heidepriem, K. Kuan,
Dr. S. Afshar V., Prof. T. M. Monro
Institute for Photonics & Advanced Sensing
School of Chemistry & Physics
University of Adelaide
Adelaide, SA 5005, Australia
E-mail: matthew.henderson@adelaide.edu.au
Dr. B. C. Gibson, Dr. J. O. Orwa, Dr. S. Tomljenovic-Hanic,
Dr. A. D. Greentree, Prof. S. Prawer
School of Physics
The University of Melbourne
VIC 3010, Australia
Dr. I. Aharonovich[+]
School of Physics
The University of Melbourne
VIC 3010, Australia
[+] Present adress: School of Engineering & Applied Science,
Harvard University, Cambridge, MA 02138, USA
DOI: 10.1002/adma.201100151
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a cavity to the emitter by fine adjustment of the cavity refrac-
tive index.[5,6] There are mature fabrication techniques for
transforming tellurite glass into optical fibers,[4] including the
well-developed field of soft glass microstructured optical fibers
(MOFs).[3] Soft glass MOF technology enables great flexibility
in tailoring linear and nonlinear optical properties through the
choice of glass materials and structure.[3] Furthermore, the glass
is fluid enough at 700 °C to consider dispersing nanodiamond
(ND), because at this temperature minimal diamond oxidation
occurs.[7]
Optical waveguides are the ideal medium for enabling com-
munication over large distances and optical channels enable
immediate applications such as quantum key distribution,
lithography and metrology.[8,9] The required platforms should
be robust, ideally solid state and room temperature compat-
ible. Color centers in diamond, and in particular the negatively-
charged nitrogen-vacancy color center (NV−), have been shown
to be capable of meeting all of these requirements.[2]
Despite the promise of the NV− center, there are significant
challenges in practical, integrated diamond nanophotonics.
One approach is to combine the emission of color centers with
conventional optical media. Examples have been attaching[10] or
growing[11] ND particles onto fiber end-faces, nanopositioning
of ND onto optical structures,[12–15] and coupling centers to
resonators,[16,17] cavities[18] and plasmonic devices.[19–21] These
hybrid approaches have by necessity used evanescent fields to
couple the emitters to the optical structures. They allow the spe-
cific placement of diamond nanocrystals on the surface of the
structure. However, they require labor-intensive post-processing
of the device, such as diamond crystal nanoplacement. Another
approach is to create monolithic diamond structures,[22–25]
which avoids interface issues, provides access to the highest
quality centers, and allows strong coupling by incorporating the
emitter in the maximum of the bound optical mode. The design
and application of such structures has recently been reviewed.[2]
However, diamond fabrication is immature compared with
more traditional optical platforms, and is yet to reach the state
of the art in, for example, silicon photonic devices.
Here we present a new methodology for combining quantum
emitters with photonic structures. In particular, we have for the
first time dispersed optically active NDs in glass, and shown
quantum emission following a fiber draw process. In this case
we have used tellurite glass. This method provides complete
encapsulation of the emitter and a platform that is easily inte-
grated into fiber-based systems. By encapsulating the emitter,
our approach allows the possibility to couple the emitter to a
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Figure 1. a) Schematic representation of the optical characterization of a
ND (containing a single photon source) embedded within a bare unstruc-
tured tellurite fiber. b,c) Tellurite billets containing ND with concentra-
tions of (b) 28 mg in 100 g tellurite and (c) 0.94 mg in 100 g tellurite. Note
that the brownish color of the glasses is due to scattering from the NDs.
d) Optical microscopy image of tellurite unstructured fiber containing
ND. The diameter of the fiber is 160 μm. e) SEM image of tellurite micro-
structured fiber showing a core suspended by thin struts in an air cladding
region, with an outer jacket of tellurite for structural strength. The core
and strut regions contain ND. Inset: zoomed image of the core region.
bound mode in a hybrid photonic structure, rather than the
evanescent coupling achieved to date. This material allows the
embedding of diamond during the fabrication of the device,
removing the need for post-processing inclusion steps. Dia-
mond in tellurite therefore constitutes a new hybrid platform
for quantum photonics applications which can realistically be
expected to be significantly more practical than previous plat-
forms, through the use of conventional soft glass fabrication,
and opens new vistas in integrated quantum devices. A sche-
matic representation of the optical characterization of a single
ND quantum emitter embedded in an optical fiber is shown in
Figure 1a.
We have fabricated bare (unstructured) and microstructured
tellurite fibers, both containing NDs, shown in Figure 1d and 1e
respectively. Fiber fabrication involves three steps: fabrication of
a glass billet, an intermediate reshaping to form a preform and
drawing of this preform into a fiber in a fiber drawing tower.
The glass melt was undertaken in two stages which were
performed at different temperatures in order to minimize dia-
mond oxidation. Raw materials, without NDs, were batched and
melted at 900 °C to create a defect-free and well-homogenized
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tellurite melt. The temperature was then reduced to 700 °C and
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NDs (NaBond nanodiamond by non-detonation process, purity
>99.95% (Grade A), average particle size 40–50 nm) were added
to the tellurite melt. 700 °C was found to be the lowest tempera-
ture at which the glass viscosity allowed both good dispersion of
the NDs and the ability to cast the molten glass in order to form
a cylindrical billet for the fiber fabrication. In this case we have
not controlled the dispersion of the NDs via established glass
melt homogenization techniques such as the use of a mechanical
stirrer. The glass melt was agitated manually and this was suffi-
cient to disperse the ND throughout the glass, although aggre-
gation was observed (as can be seen in later confocal images).
Processing time at this temperature was minimized to reduce
the oxidation of diamond.[7] We have produced tellurite billets
using this fabrication process with varying concentrations of
ND. An example of two diamond-containing billets are shown in
Figure 1b and 1c for ND concentrations of 28 mg and 0.94 mg
ND powder in 100 g tellurite, respectively.
We used an extrusion technique[26] to fabricate preforms
from a billet. In the case of the unstructured fiber this pre-
form is a 10 mm diameter tellurite-ND rod and for micro-
structured fiber a more complex preform is extruded, reduced
in diameter, and then inserted into an undoped tellurite tube.
Extrusion was chosen to fabricate the fiber preform over other
techniques, such as casting, because of a low processing tem-
perature (350 °C) and the freedom to fabricate structured fiber
geometries, such as the fiber shown in Figure 1e. Billets of var-
ying ND concentration were used for the fiber fabrication and
subsequent characterization. Preforms were drawn down to a
final fiber at 400 °C in a fiber drawing tower. Fibers with outer
diameters as small as 160 μm were fabricated.
Raman and photoluminescence (PL) spectra of a high
ND concentration (28 mg ND in 100 g tellurite) rod preform
were measured, as shown in Figure 2a and 2b respectively,
confirming the presence of ND in the fiber preform. These
were compared with the 40 nm ND powder and an undoped
tellurite glass sample. The absence of graphitic Raman fea-
tures (G peak) in the preform is likely due to more rapid oxi-
dation of the graphitic sp2 bonds compared to the diamond
sp3 bonds. Similar results were reported previously in 55 nm
ND,[27] where the Raman G peak decreased by a factor of 10
after 20 min of oxidation at 400 °C. During glass fabrication
the 700 °C melt temperature is well above the 400 °C oxidation
temperature of graphite,[27] while being only slightly above the
670 °C oxidation temperature of diamond.[7] Note that as the
Raman cross-section of graphite is ∼50 times larger than that
of diamond, the graphitic peak in the ND spectra denotes only
a small percentage of graphite and the lack of such a peak in
the preform is a strong indicator of an absence of graphite in
this sample. PL spectra show that while both the ND powder
and the ND-doped preform show NV− and NV0 (the neutrally-
charged nitrogen-vacancy color center) luminescence peaks, the
undoped tellurite glass sample shows no PL over the NV emis-
sion window. The PL zero-phonon line (ZPL) for NV− and NV0
are marked in Figure 2b.
The negative charge state of the NV color center is desir-
able as it shows spin polarization and long coherence time
even at room temperature.[2] In Figure 2c, we show the ratio
of NV− to total NV as a function of excitation power for both
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Figure 2. Raman and PL spectra obtained at 80 K from 40 nm diamond
powder, a high ND concentration (28 mg ND in 100 g tellurite) tel-
lurite fiber preform sample and an undoped tellurite glass sample.
a) Raman spectra showing the first-order diamond Raman line for the ND
powder (red) and the ND-doped tellurite preform sample (blue). Note
the absence of pronounced graphitic features (G peak in ND data) in the
tellurite glass which is possibly due to selective oxidation of the ND sp2
bonds, compared with the sp3 bonds. b) PL intensity spectra. D1 and G
refer to 1st order diamond Raman line and graphite peak, respectively, in
the ND powder (red). NV0 and NV− peaks can be observed in both the
ND powder (red) and ND-doped tellurite preform sample (blue) data.
The undoped tellurite (green) exhibits no significant fluorescence over
the PL range of the NV− centers. c) Ratio of NV− to total NV as a function
of excitation power for both the ND powder (red) and the ND in tellurite
preform (blue).
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the ND powder and the ND in tellurite preform. We obtain a
factor of 1.7 increase in the fraction of NV− to total NV in the
ND in tellurite preform compared with the ND powder. This
data is calculated by the ratio of the integrated NV− and NV0
peaks in the PL spectra. As such this is an average sampling
of the NDs present in the glass and powder and so this result
is a statistical indication, similar to that in.[28] The ND powder
used to measure the Raman and PL spectra is from the same
batch of materials used in the fabrication of the hybrid tellurite
glass. This enhancement is thought to be due to removal of
sp2 carbon and termination of the diamond surface by oxygen-
containing functional groups and is in agreement with the
improvements seen in oxygen terminated single crystal dia-
mond by Fu et al.[29] These results indicate that the color center
properties are improved compared with ND powder as a result
of undergoing the glass and fiber fabrication processes.
We have confirmed the presence of NDs containing NV
color centers embedded in the drawn unstructured fibers using
confocal microscopy. Room temperature scanning confocal
microscopy was used to investigate the single-photon emission
characteristics of the fiber-embedded diamond color centers.
Fiber samples were cleaved to reveal a pristine cross-section.
Two 60 μm × 60 μm confocal fluorescence intensity maps are
shown in Figure 3a and 3b for fibers fabricated from 28 mg ND
and 0.94 mg ND in 100 g tellurite billets, respectively. The exci-
tation focal point was 5 μm below the surface, guaranteeing that
embedded emitters were addressed. The signal was filtered to
measure NV− center emission only using a bandpass filter from
650 to 750 nm. The edge of the fiber is clearly visible in both
confocal scans. Each fluorescent point corresponds to emission
from either individual or small agglomerations of NDs, which
may contain (in principle) several NV− centers.
Image particle counting software (ImageJ) was used to esti-
mate the final ND concentration. The fluorescent particles were
counted from the confocal images and divided by the volume
of the fibre sampled, assuming a 0.5 μm focal depth. Values of
∼1.8 × 1010 cm−3 and ∼1.5 × 1011 cm−3 were calculated for fibers
with 0.94 mg and 28 mg ND in 100 g tellurite respectively. This
gives an estimated embedded particle yield of approximately
4.5% and 1.5% for 0.94 mg and 28 mg ND in 100 g tellurite
respectively, if we make the assumption that the ND mass
added is comprised only of fluorescent 40 nm spherical ND.
This estimate is clearly a conservative lower bound on the yield
as there will be the addition of non-fluorescent ND particles,
uncertainty in the mass of ND incorporated into the glass due
to accumulation on the melting crucible wall during addition to
the melt, and aggregation of the particles causing a decrease in
the measured particle count in the confocal images (which is
much more pronounced in the 28 mg ND sample). Photon sta-
tistics from each fluorescent region on the confocal map were
studied to identify single NV− color centers.
Fluorescent emitters embedded in the tellurite were found
to exhibit a characteristic single photon dip in the second order
correlation function at the zero delay time (t = 0). The photon
statistics of a single NV− color center embedded in the endface
of the sample shown in Figure 3a were measured at room tem-
perature with 1 mW excitation power at λ = 532 nm and are
shown in Figure 3c. The lowest measured value of g(2)(0) = 0.04
indicates that a single photon emitter was addressed. The solid
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Figure 3. a,b) Diamond NV− PL intensity scanning confocal maps of
60 μm × 60 μm regions of cleaved unstructured tellurite fiber endfaces.
Fibers were fabricated from billets with (a) 28 mg ND and (b) 0.94 mg
ND in 100 g tellurite. The excitation focal point was 5 μm below the
surface. c) Background corrected second order autocorrelation function
(blue circles) of a single NV− center (the value of g(2)(0) = 0.04 indicating
single-photon emission) embedded in the endface of the 28 mg ND in
100 g tellurite optical fiber, shown above, measured at room tempera-
ture. The solid red line represents a single exponential fit of the photon
statistics. d) Background corrected photo-luminescence spectrum, col-
lected for 60 seconds at room temperature, of the single photon emitter
measured in (c).
red line in Figure 3c represents a single exponential fit of the
photon statistics. The measured single photon emission rate was
∼45 k counts s−1 under the same excitation conditions. The emis-
sion rate from this center is similar to that obtained from single
centers in bulk diamond.[25] The background from the tel-
lurite in a region without ND was ∼5 k counts s−1, indicating
a very low background comparable with that measured for ND
on silica.[12] Figure 3d shows the background corrected photo-
luminescence spectrum, collected for 60 seconds at room
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temperature, of the single photon emitter measured in Figure 3c.
The spectrum is typical of the emission from a single NV− color
center at room temperature which shows the NV− zero phonon
line at 637 nm and the broad NV− phonon side band.
We have engineered a new hybrid material by incorporating
NDs containing single nitrogen-vacancy color centers into tel-
lurite glass. This technology is a radical departure from con-
ventional approaches of evanescent coupling diamond with
photonic devices, and it allows the tailoring of strong inter-
actions between the bound mode fields of the structure and the
diamond color centers. We observed single photon emission
from the embedded NDs. We also found a factor of 1.7 increase
in the NV− to total NV ratio for the ND incorporated in tellurite
preform compared with the ND powder. By incorporating NV
containing ND in a soft glass, we have fabricated an important
hybrid material with implications for quantum information
processing and quantum key distribution schemes. Although
we have concentrated on NV− centers, there are now many dis-
tinct diamond single photon emitters[30,31] which, due to the
large transparency of the tellurite, are all candidates for glass
incorporation. This combination of advanced photonics and
quantum emission promises a new era of quantum sensors
and more practical quantum information processing.
Experimental Section
Glass fabrication: Tellurite glass was made by batch melting TeO2,
ZnO, La2O3 (99.99% purity) and Na2CO3 (99.997% purity) using a
gold crucible in a controlled atmosphere furnace using a mixture of
dry nitrogen and oxygen at 900 °C. The chemical composition of the
tellurite glass was 2.2La2O3-4.9Na2O-19.6ZnO-73.3TeO2 (mol%).
Temperature was reduced to 700 °C and NDs (NaBond nanodiamond
by non-detonation process, purity >99.95% (Grade A), average particle
size 40–50 nm) were added to the melt. Theoretical ND densities for the
samples containing 0.94 mg and 28 mg of NDs added to 100 g tellurite
melt are approximately 4 × 1011 cm−3 and 1 × 1013 cm−3, respectively.
The crucible was returned to the furnace at 700 °C for approximately
15 minutes to disperse the NDs, removed and cast into a cylindrical
brass mold. The billets were annealed at 295 °C for 2 h and then cooled
to room temperature at a rate of 0.2 °C min−1. Final billet dimensions
were approximately 25 mm height × 30 mm diameter. Billets had a final
mass of 98 g.
Preform fabrication and fiber drawing: The glass billets were extruded[26]
by a ram with a furnace temperature of 355 °C through a stainless steel
die with a ram speed of 0.2 mm min−1 to produce fiber rod preforms
with diameters of 10 mm and lengths of 160 mm. The ram force was
varied to maintain a fixed ram speed and was approximately 3–3.5 kN
during the extrusion. The preforms were annealed at 310 °C for 2 h and
cooled to room temperature at a rate of 0.2 °C min−1. Fiber preforms
were drawn at a temperature of 400 °C into fibers with a target outer
diameter of 160 μm using a soft glass fiber drawing tower.
Raman and PL of preform: Raman and PL spectra were measured
at 80 K using the 514.5 nm line of an argon ion laser as the excitation
source. The beam was focused to a 1 μm spot using a 50× objective
of a Leica DMLP microscope. The backscattered signals were collected
through the same objective and analyzed by a Renishaw Raman
spectrometer fitted with a cooled CCD array detector.
Acknowledgements
T.M.M. acknowledges the support of an ARC Federation Fellowship
(project number FF0883189). S.T-H. is supported by the ARC Australian
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Research Fellowship (project number DP1096288). A.D.G. acknowledges
the support of an ARC QEII Fellowship (project number DP0880466).
The authors acknowledge that the original concept for embedding
quantum-based emitters in optical fibers made from glasses drawn
at low temperatures was also contributed by Shane Huntington,
Paul Mulvaney and Simon Fleming. We also acknowledge Alastair Dowler
and Roger Moore for fiber drawing, and David Simpson for helpful
discussions.
Received: January 14, 2011
Revised: February 28, 2011
Published online: April 21, 2011
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