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Homoepitaxial Growth of Single Crystal Diamond
Communication
Membranes for Quantum Information Processing
Igor Aharonovich,* Jonathan C. Lee, Andrew P. Magyar, Bob B. Buckley, Christopher G. Yale,
David D. Awschalom, and Evelyn L. Hu
Fabrication of devices designed to fully harness the unique
properties of quantum mechanics through their coupling
to quantum bits (qubits) is a prominent goal in the field of
quantum information processing (QIP). Among various qubit
candidates,[1] nitrogen vacancy (NV) centers in diamond have
recently emerged as an outstanding platform for room tem­
perature QIP.[2–5] However, formidable challenges still remain
in processing diamond and in the fabrication of thin diamond
membranes, which are necessary for planar photonic device
engineering. Here we demonstrate epitaxial growth of single
crystal diamond membranes using a conventional microwave
chemical vapor deposition (CVD) technique.[6] The grown
membranes, only a few hundred nanometers thick, show bright
luminescence, excellent Raman signature and good NV center
electronic spin coherence times. Microdisk cavities fabricated
from these membranes exhibit quality factors of up to 3000,
overlapping with NV center emission. Our methodology offers
a scalable approach for diamond device fabrication for photo­
nics, spintronics, optomechanics and sensing applications.
The exceptional properties of diamond, including a wide
electronic and optical band gap, excellent thermal conductivity,
and its biocompatibility are attractive for numerous optoelec­
tronic and sensing applications.[6] One diamond color center in
particular, the negatively charged nitrogen vacancy (NV) center,
is among the most promising solid state qubits due to its room
temperature operation, long spin coherence time, and suit­
ability for optical initialization and readout.[7] Embedding color
centers within a single crystal diamond membrane enables
promising applications, including diamond-based QIP.[8,9] To
this end, optically–active thin membranes are essential, as they
are the fundamental building blocks of photonic components
such as microcavities, photonic crystal cavities, resonators and
waveguides.
Fabrication of planar devices often requires the material be
undercut to achieve optical, electrical or mechanical isolation,
as in the formation of mechanically-sensitive cantilever devices,
Dr. I. Aharonovich,[+] J. C. Lee,[+] Dr. A. P. Magyar, Prof. E. L. Hu
School of Engineering and Applied Sciences
Harvard University, MA 02138, USA
E-mail: igor@seas.harvard.edu
B. B. Buckley, C. G. Yale, Prof. D. D Awschalom
Center for Spintronics and Quantum Computation
University of California
Santa Barbara, California, 93106, USA
[+] I.A. and J.C.L. contributed equally to this work.
DOI: 10.1002/adma.201103932
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optical microdisk cavities, or photonic crystal cavities.[10–12] Such
structures are often formed by incorporating a sacrificial layer
into the initial bulk material structure. Selective etch removal
of the sacrificial layer can then create an undercut structure, or
a larger membrane with thickness of tens to hundreds of nano­
meters, depending on the device application. However, such an
approach is not available for creating undercut or membrane
structures in diamond, as high quality hetero-epitaxy of single
crystal diamond on dissimilar substrates has not yet been dem­
onstrated due to lattice mismatches and low surface diffusion
of carbon atoms.[6,13,14]
An alternative technique has been employed for diamond:
high energy (∼1–3 MeV) and high dose ion implantation
(∼1 × 1017 ions/cm2) generates a thin amorphous layer below
the diamond surface that can be selectively etched leaving
behind a diamond membrane several hundred nanometers
in thickness.[15–21] Nevertheless, poor spin coherence proper­
ties, weak luminescence from its color centers, and a residual
built-in strain as a result of the high ion damage significantly
limit the performance of diamond membranes fabricated in
this manner. Indeed, no working optical cavities, spin measure­
ments or devices have been demonstrated from ion-damaged
diamond membranes to date.
To address this challenge, we introduce an approach that
utilizes the diamond membranes as templates for the epitaxial
overgrowth of a thin layer of single crystal diamond. Growth
is carried out in a plasma-enhanced chemical vapor deposition
(PECVD) reactor and results in single crystal diamond layers
with superior physical, optical, and spin properties than their
original diamond templates. Furthermore, the overgrowth
process allows us to intentionally dope the diamond device
layer with color centers such as NV or silicon-vacancy (SiV)
centers that were not present in the original diamond template.
Indeed, strong luminescence, narrow Raman peaks and the
appearance of NV center spin lifetimes in the membrane, are
characteristic of a good quality bulk diamond. After growth,
the diamond template can be completely etch-removed, leaving
the highest quality overgrown diamond membrane to be fur­
ther formed into device structures (see experimental methods).
The schematic of the process is depicted in Figure 1a. The spe­
cific homoepitaxial growth conditions were: microwave power
950 W, pressure 60 Torr under 400 standard cubic centimeters
per minute of 99:1 CH4/H2. We note that our growth conditions
are not typical of those used for homoepitaxial, single crystal
diamond growth, which often requires higher microwave power
densities (∼2–4 kW) and higher pressure (∼150–250 Torr).[22,23]
Figure 1b,c show the top view and the cross sectional
scanning electron microscope (SEM) images of the original
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Figure 1.  (a) Schematic illustration of the regrowth process of the diamond membrane using a
PECVD reactor. (b) SEM side view and (c) top view of the original diamond membrane before
the regrowth. (d) SEM side view and (e) top view showing a ∼300 nm overgrowth of a single regrown membranes showed bright fluores­
crystal diamond. The pits observed on the surface are transferred from the original membrane. cence even though the original templates
(f) AFM scan of a 5 μm strip demonstrating the smoothness of the top membrane surface. The
surface roughness is measured to be 4 nm.
membrane, 1.7 μm in thickness. Figure 1d,e illustrate the over­
grown material after 5 minutes of growth. The single crystal
material, with a top (100) facet, is clearly observed on top of
the original membrane. No indications of polycrystalline mate­
rial, grain boundaries or surface defects (e.g., hillocks) are
observed. The pits in the regrown layer are transferred from
the original membrane, which was pitted. In principle, this can
be avoided through the use of smooth, dislocation free, single
crystal diamond as a starting material. Importantly, the undam­
aged regions of the regrown material are very smooth. Atomic
force microscope (AFM) scans reveal that the root mean square
(RMS) surface roughness is only 4 nm (Figure 1d). In com­
parison, the RMS surface roughness of a typical commercially
available CVD single crystal diamond (Element Six, Inc) is on
the order of 2–3 nm.
Raman spectroscopy can provide detailed information about
the structural quality of a material (see experimental methods).
The best diamond templates show Raman peaks at 1331 cm−1
with a FWHM of 9.9 cm−1 (after removing the most dam­
aged region but before any annealing or regrowth treatment).
For comparison, the Raman peak we measure for bulk single
crystal diamond is centered at 1333.5 cm−1 with a FWHM of
2.3 cm−1. Remarkably, the Raman signature of the composite
overgrown membrane-plus-template gave a peak value of
1332 cm−1 with a FWHM of 6.6 cm−1. These values are a con­
volution of the Raman peak from the overgrown material with
that of the membrane template, and accounts for the best fit to
two peaks, shown in Figure 2a.
To further gauge the influence of the template quality on
the properties of the overgrown diamond, material was over­
grown on the most heavily-damaged surface of the template
(which was not removed by etching) (Figure 2b).[19] Even with a
heavily damaged template material, the epitaxially grown mate­
rial exhibits superior Raman characteristics with linewidth of
∼ 3 cm−1, approaching the quality of a bulk single crystal dia­
mond, despite the shifted and much broader Raman signature
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of the template, as seen in the green curve
Communication
of Figure 2b. This is convincing evidence
that the overgrown diamond film has much
improved structural properties over its
highly-damaged, highly-strained diamond
template. This is contrary to conventional
epitaxial growth of other semiconductors
(e.g., GaAs) where the strain in the tem­
plate is manifested in the properties of the
overgrown material and often reduces its
quality.[24] However, strain fields do exist in
our grown material, as is evident by the opti­
cally detected magnetic resonance (ODMR)
measurements (shown below).
To further investigate the optical properties
of the regrown material, photoluminescence
(PL) measurements were recorded under
532 nm excitation at room temperature. The
were not optically active. The appearance
of PL clearly indicates that the formation of
color centers occurs during the CVD growth.
We have demonstrated this by engineering two types of different
membranes–one with primarily NV centers and the other with
SiV centers. The PL of these membranes is presented in Figure 3.
The impurity incorporation can be controlled by placing the
template on various substrates, e.g., silicon or other bulk dia­
mond. We believe that during the growth the plasma slightly
etches the substrate, whose elements are subsequently incorpo­
rated into the growing diamond lattice.[25] No nitrogen gas was
intentionally introduced during the growth; the nitrogen source
is due to residual nitrogen in the chamber.
Some of the most promising scientific and technological
applications of diamond are spin-based QIP algorithms[3,4] and
detection of weak magnetic fields with high sensitivity.[26–29] For
these, an important prerequisite is characterizing the coherent
dynamics of the NV center electron spin. We note that no
electron spin resonance signal was detected from the original
diamond templates prior to the regrowth process. After the
epitaxial regrowth of membranes containing NV centers, an
ODMR signal was observed, motivating further investigation of
the NV center spin properties within the grown membranes.
Figure 4 plots various measures of ensemble spin coherence
as functions of time at room temperature and with no applied
magnetic field. More details regarding the timing sequences
to determine these measures can be found in the Supporting
Information. In Figure 4a, the NV center longitudinal spin
coherence as a function of time is plotted. Fitting to an expo­
nential decay reveals a spin-lattice relaxation time of T1 = 5 ms
for the NV center ensemble. The transverse homogeneous spin
coherence, plotted in Figure 4b, was measured with a Hahn echo
sequence and was found to have a value of T2 = 3.5 μs when
fit to a single exponential decay. Figure 4c plots the transverse
inhomogeneous spin coherence, taken with a Ramsey sequence
(off resonance by ∼25 MHz). The pronounced beating in the
Ramsey data suggests several distinct spin resonance frequen­
cies which may be due to crystal strain energetically splitting
the SX and SY spin sublevels as well as a small stray magnetic
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Communication
Figure 2.  (a) Diamond membrane grown on a lifted-off diamond slab
with the damaged side etched away. The double Voigt fitting of the Raman
line (red curve) reveals a FWHM of ∼4 cm−1 for the regrown material
(blue curve) and ∼7 cm−1 for the original membrane (green curve).
(b) Diamond membrane growth on the damaged side of the lifted-off
membrane. Despite the damaged original material with a wide Raman line
(green curve, FWHM of ∼17 cm−1), the regrown material shows a much
narrower FWHM of ∼3 cm−1 for the regrown material (blue curve).
field. A fit consisting of a single exponential decay envelope
around four beating frequencies reveals T2∗ = 158 ns for this
ensemble of NV centers. It should be noted that transverse spin
coherence is sensitive to the surrounding spin bath, originating
from the presence of other electron and nuclear spins as well
as magnetic fluctuations on the surface. The measured values
of T2 and T2∗ for the regrown material are comparable with
both natural NVs in type Ib diamond[28] and shallow implanted
NVs in a high purity bulk diamond[30,31] (T2 ∼1–20 μs) and are
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Figure 3.  (a) PL spectrum recorded from an overgrown membrane, with
dominating NV concentration. (b) PL spectrum recorded from a different
overgrown membrane, showing primarily the SiV defects.
higher than typical coherence times found in nanodiamonds (T2
∼1 μs).[32] Nevertheless, it is still shorter than the isotopically
pure single crystal diamond (T2 ∼ 2 ms).[7]
Remarkably, good spin behavior exists in the regrown mate­
rial despite the fact that the original template did not show any
ODMR signal and the regrown membrane is only a few hun­
dred nanometers thick. The spin properties of the regrown
membrane further confirm the good quality of the thin, single
crystal diamond membrane and indicate promise for applica­
tions in nano-magnetometry and QIP.
The spin properties of the regrown diamond membranes
can be significantly improved by growing material in a purer
environment, resulting in fewer paramagnetic defects such as
substitutional nitrogen. Additionally, growing with 12C isotopi­
cally purified methane has the promise to achieve millisecond
T2 coherence times, as the nuclear spin of 13C can significantly
reduce the NV spin coherence.[7] Furthermore, additional
experimental steps such as high temperature annealing[31] may
also improve the coherence times of NV centers in the grown
material.
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The regrowth results are intriguing for

Communication
a number of reasons. First, an improved
Raman signature indicates a much smaller
strain distribution in the regrown mem­
branes. This is despite the fact that the orig­
inal templates are structurally imperfect with
high strain fields. Second, the regrown mate­
rial exhibits good spin properties, unlike the
original template which did not exhibit any
spin signature. Third, the regrowth meth­
odology allows engineering of other color
centers within the regrown material. Fur­
ther exploration of the growth conditions
could lead towards thin single crystal dia­
mond membranes with a low distribution
of color centers that can emit single photons
on demand (e.g., NV, SiV, Cr) – an impor­
tant prerequisite for single photon device
engineering.
The successful homoepitaxial growth of
thin diamond membranes is a pivotal step in
advancing diamond processing. Our results
provide important insights that can poten­
tially further the understanding of the com­
plicated diamond CVD growth, particularly
its nucleation steps. The demonstration of
good quality epitaxial diamond growth even
on damaged diamond template opens new
avenues towards engineering of thin, single
diamond membranes. The scalability of this
process can propel the use of diamond from
laboratory setting into a plethora of devices
spanning high power electronics, photonics,
sensing and QIP.

Experimental Section
Figure 4.  (a) Spin lattice relaxation time, yielding T1 ∼ 5 ms. The red curve is a single expo- Generation of initial diamond templates: A type IIA
nential fit of the data. (b) Hahn-echo sequence of the transverse homogeneous spin coher- CVD diamond crystal (Element Six) was implanted
ence time resulting with a T2 ∼ 3.5 μs. The red curve is a single exponential fit of the data. with He ions (1 MeV, 5 × 1016 He/cm2) to create
(c) Ramsey sequence to determine transverse inhomogeneous spin coherence precession a damage layer and annealed for one hour at
decay time, yielding T2∗ = 158 ns. Error bars are smaller than data markers. The sequences 900 °C.[19] The sample was then immersed in water,
applied to measure the spin properties are schematically depicted. All the data are recorded at and using electrochemical etching carried out
room temperature with no applied magnetic field. under constant voltage, the membranes were lifted
off and placed on different substrates. The original
templates have (100) crystallographic orientation,
Having at our disposal an optically-active, thin, single crystal same as the original type IIA diamond crystal.
diamond membrane, we demonstrate its suitability for QIP by Regrowth process– the original single crystal diamond membranes
were first cleaned using a mixed (1:1:1 sulfuric–perchloric–nitric
fabricating an optical microcavity. Figure 5a shows PL spectra
acid) and put into a Seki Technotron AX5010-INT PECVD reactor. The
recorded from a microdisk (black curve) and the substrate (red chamber was evacuated below 0.1 mTorr and flushed with H2 gas. After
curve) at room temperature. The NV zero phonon line (ZPL) is the plasma ignition (only hydrogen ambient), it took approximately
visible at 637 nm. The peaks decorating the PL recorded from 8 minutes for the temperature and the pressure to stabilize, at
the microdisk are the modes with quality factors (Q) ∼1500. which time the methane was introduced. The homoepitaxial growth
Q’s of up to 3000 were measured from the microdisk cavities. conditions were: microwave power 950 W, pressure 60 Torr, 400 SCCM
Figure 5b shows a typical SEM image of a microdisk cavity of 99:1 CH4 (99.999%)/H2(99.999%) for 5 minutes. No external
heating source was used and the temperature was ∼850 °C as read by
(diameter of 2.5 μm and a thickness of ∼800 nm), fabricated a pyrometer.
from the epitaxially-grown membrane. Device fabrication: the regrown membranes were flipped and thinned
In conclusion, we have described a process that produces thin, down using oxygen inductive coupled plasma reactive ion etching
optically-active, high-quality single crystal diamond membranes. (ICP-RIE) to their final thickness of ∼500 nm. A silicon dioxide hard mask

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Communication
Figure 5.  (a) PL spectra recorded from the diamond membrane (red
curve) and from a 1 μm microdisk (black curve, shifted for clarity)
under 532 nm excitation at room temperature. The ZPL of the NV
center is clearly seen at 637 nm. The spectrum from the microdisk is
decorated with modes with typical Q ∼1500. (b) A typical SEM image
of a microdisk cavity with a diameter of 2.5 mm and a thickness of
∼800 nm.
was deposited on top of the membranes and the microdisk cavities were
patterned using e-beam lithography and etched down using ICP-RIE.
Spectroscopy: the Raman data was collected using 532 nm laser
excitation with a conventional confocal Raman microscope (LabRAM
ARAMIS, Horiba Jobin-Yvon) at room temperature. The typical spatial
resolution of the microscope is ∼1 μm.
The PL measurements were recorded using a custom built confocal
microscope using a 532 nm continuous wave (CW) diode laser through
a 100×, 0.9 numerical aperture objective. The emission was collected
through the same objective and directed into a spectrometer. The laser
light was filtered using a dichroic mirror.
Spin coherence measurements: The samples were placed in a confocal
microscopy setup with a 100× objective where a 532 nm laser for
photoexcitation, microwave magnetic fields for spin manipulation, and
the sample PL measured by an avalanche photodiode were all gated in
time for time-domain spin coherence measurements. Timing sequences
for the measurements of T1, T2, and T2∗ (see Supporting Information)
were generated by an arbitrary waveform generator.
Supporting Information
Supporting Information is available from the Wiley Online Library or
from the author.
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Acknowledgements
The authors thank Prof David Clarke for the access to the Raman
facilities, F.J. Heremans and A.L. Falk for the assistance with the optical
measurements, M. Huang for the assistance with ion implantation.
The authors also acknowledge A. Yacoby, M. Grinolds, S. Hong and
P. Maletinsky for the assisting with the initial ESR measurements and
thank T.M. Babinec for useful discussions. The financial support from
DARPA, QuEST and AFOSR is gratefully acknowledged.
Received: October 12, 2011
Revised: October 22, 2011
Published online: January 31, 2012
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