Direct observation and mechanism for enhanced field emission sites in platinum ion

implanted/post-annealed ultrananocrystalline diamond films

Kalpataru Panda, Kamatchi J. Sankaran, Eiichi Inami, Yoshiaki Sugimoto, Nyan Hwa Tai, and I-Nan Lin
Citation: Applied Physics Letters 105, 163109 (2014); doi: 10.1063/1.4898571
View online: http://dx.doi.org/10.1063/1.4898571
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APPLIED PHYSICS LETTERS 105, 163109 (2014)

Direct observation and mechanism for enhanced field emission sites in

platinum ion implanted/post-annealed ultrananocrystalline diamond films
Kalpataru Panda,1,a) Kamatchi J. Sankaran,2 Eiichi Inami,1 Yoshiaki Sugimoto,1
Nyan Hwa Tai,2 and I-Nan Lin3,b)
1

Graduate School of Engineering, Osaka University, 2-1, Yamada-Oka, Suita, Osaka 565-0871, Japan
Department of Materials Science and Engineering, National Tsing Hua University, Hsinchu 30013, Taiwan
3
Department of Physics, Tamkang University, Tamsui 251, Taiwan
2

(Received 29 August 2014; accepted 20 September 2014; published online 24 October 2014)
Enhanced electron field emission (EFE) properties for ultrananocrystalline diamond (UNCD)
films upon platinum (Pt) ion implantation and subsequent post-annealing processes is reported,
viz., low turn-on field of 4.17 V/lm with high EFE current density of 5.08 mA/cm2 at an applied
field of 7.0 V/lm. Current imaging tunneling spectroscopy (CITS) mode in scanning tunneling
spectroscopy directly revealed the increased electron emission sites density for Pt ion implanted/
post-annealed UNCD films than the pristine one. The high resolution CITS mapping and local
currentvoltage characteristic curves demonstrated that the electrons are dominantly emitted
C 2014 AIP Publishing LLC.
from the diamond grain boundaries and Pt nanoparticles. V
[http://dx.doi.org/10.1063/1.4898571]
Carbon and related materials have received great attention from research community due to their immense potential
to be employed as a cold cathode material in flat panel displays and electron field emitting devices.13 Among field
emitting materials, diamond is known as a fascinating electronic material due to its negative electron affinity (NEA) surface and low effective work function.4,5 Ultrananocrystalline
diamond (UNCD) film is a special form of diamond film that
has recently attracted broad interest because of its exclusive
granular structure and better electron field emission (EFE)
properties.6,7 The fact that diamond or UNCD films can be
used as a material for the fabrication of cold cathode or other
electron emitting devices require the film to be conductive.
The incorporation of N2 during the UNCD films growth
plasma can effectively improve the electrical conductivity and
the EFE properties of the films.810 This is due to the conversion of an amorphous carbon (a-C) phase to a graphitic phase
at the grain boundaries that increases the number of conductive grain boundary channels on the surface.8,9,11 It indicates
that the grain boundary conduction mechanism is responsible
for the observed increase in EFE properties of N2 doped
UNCD films,12,13 while nano-sized diamond grains play a little role. However, a very high temperature of about 800  C is
required for the synthesis of N2 doped UNCD films.12,13
On the other hand, ion implantation can modify the
properties of materials through controlled doping of variety
of dopants.14,15 Ion implantation can introduce defects and
break the CC and hydrocarbon bonds to form sp2 carbon
and can be used to tailor the sp2/sp3 ratio for the diamond or
related carbon materials by properly selecting the energy and
dose of implantation.16,17 The sp2-bonded carbon phase in
the diamond grain boundaries can be thought to be the prime
electrical conduction promoters, which form interconnected
networks of conducting sp2 path, where electrons can easily
move. However, the electrical conductivity of a-C phases
a)

Electronic mail: panda@afm.eei.eng.osaka-u.ac.jp/phy.kalpa@gmail.com

Electronic mail: inanlin@mail.tku.edu.tw

b)

0003-6951/2014/105(16)/163109/5/$30.00

contained in the grain boundaries of UNCD films is not sufficiently high and therefore, limits the EFE properties achievable for UNCD films.12,13,18 Converting the a-C phase to
graphitic phase seems to be the right way for further improving the EFE properties of UNCD films.
Moreover, the direct detection of electron emission site
from the diamond grain or grain boundaries in such a microscopic scale is crucial. The grain boundary electron
emission was explained by May and co-workers19 who
intentionally used high input bias to burn out the emission
sites in polycrystalline diamond films. The damaged emission sites showed ring-like craters surrounding grains, suggesting that the grain boundaries were the electron
emission carriers that damaged due to passage of excessive
current. On the other hand, field electron emission microscopy (FEEM), is used to collect the field-emitted electrons
and image them enabling their origin to be determined.
Garguilo used FEEM20 to study the emitting sites from
NCD films and found that the emission originated from
localized regions smaller than 100 nm in size. Moreover, up
to date three experimental studies report the observation of
emission sites by using scanning tunneling microscopy
(STM) to map simultaneously the surface topography and
the emission site densities on diamond surfaces. Karabutov
et al.21 used STM to study the emission sites of microcrystalline diamond films and reported that the emission sites
were not due to the sharp morphology protrusions (grains)
but instead the morphology pits (grain boundaries).
However, it was not clear whether the diamond grain or
grain boundaries were the emission sites from the data for
one sample at 400  400 nm scale. Krauss and co-workers22
used STM to show that the emission sites from UNCD films
coated on sharp Si micro tip are related to minima or inflection points in the UNCD surface topography, and not to surface asperities. Their tight binding pseudo potential
calculations along with the STM results indicate that
the grain boundaries play a critical role in the electron
emission properties of UNCD films. Recently, Chatterjee

105, 163109-1

C 2014 AIP Publishing LLC

V

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and co-workers23 showed that the grain boundaries are the

prominent electron emission sites for NCD films by using
ambient tunneling atomic force microscopy. Moreover,
the surface deformation mediated by surface contamination
in ambient conditions affect the tunneling current and
hence the real detection of the electron emission sites.24
Moreover, it is not clear whether the grain boundaries are
the emission sites when the diamond grain size reduces to
few nanometers.23
In this letter, we report the enhanced EFE properties of
UNCD films upon Pt ion implantation and subsequent postannealing process. The direct observation of electron emission sites in Pt ion implanted/post-annealed UNCD films in a
nanometer scale are discussed by using current imaging tunneling spectroscopy in scanning tunneling spectroscopy
(STS) mode in ultra high vacuum conditions.
The UNCD films were grown on n-type silicon substrates in a microwave plasma enhanced chemical vapor
deposition (2.45 GHz IPLAS-CYRANNUS-I, Troisdorf,
Germany) system. The substrates were ultrasonicated in
methanol solution containing a mixture of diamond powders
and titanium powders (SIGMA-ALDRICH; 365 mesh) for
45 min to facilitate the nucleation process. The UNCD films
were grown in Ar (99%)/CH4 (1%) plasma (100 sccm), at
1200 W and 200 mbars for 3 h, without heating the substrates.
The 500 keV Pt ions with an ion fluence of 1  1017 ions/cm2
were implanted on UNCD films at room temperature in a
pressure below 2  10 7 mbars, followed by annealing at
800  C for 30 min. For simplicity, the pristine UNCD films
are designated as P-UNCD, whereas the Pt ion implanted/
post-annealed films as Pt&A-UNCD. The microstructure of
the UNCD films was examined using transmission electron microscopy (TEM; JEOL 2100F). Field emission measurements
were carried out in a tunable parallel plate setup, in which the
cathode (UNCD films) to anode (tip, a Molybdenum rod with
a diameter of 2 mm) distance is controlled by a micrometer
and an optical microscope. The EFE behavior was investigated
elaborately in a microscopic scale by a commercial ultrahigh
vacuum scanning tunneling microscopy (UHV-STM, 150
Aarhus, SPECS GmbH) system, at room temperature with a
base pressure of at least 5  10 10 Torr. For topographic imaging and CITS mapping, we have used tungsten tips, which
were prepared by the electrochemical etching process. CITS
spectra with voltages ramping from 3 to 3 V were measured
simultaneously during the STM imaging.
The effect of Pt ion implantation/post-annealing processes in modifying the EFE properties of UNCD films is
shown in Fig. 1. The turn-on field (E0) designated here as the
interception of the high and low-field line segments of the
F-N plots, viz., ln(J/E2) versus 1/E, is shown as inset of Fig. 1.
The Pt ion implantation/post-annealing processes improved
markedly the EFE properties of UNCD films as shown by
curve II in Fig. 1. The E0 value for the EFE process decreased
from (E0)P-UNCD 22.2 V/lm for P-UNCD films [curve I,
Fig. 1] to (E0)Pt&A-UNCD 4.17 V/lm for Pt&A-UNCD films
[curve II, Fig. 1], whereas the EFE current density (J) of
P-UNCD increased from 1.25 mA/cm2 (at an applied field of
37.1 V/lm) to 5.08 mA/cm2 for Pt&A-UNCD (at an applied
field of 7.1 V/lm). Moreover, while the P-UNCD films are
too resistive to be measured using the van der Pauw

Appl. Phys. Lett. 105, 163109 (2014)

FIG. 1. Electron field emission properties (JE curves) of (I) P-UNCD, (II)
Pt&A-UNCD films. The inset shows the corresponding Fowler-Nordheim
(F-N) plot.

configuration, the Pt&A-UNCD films show high electrical

conductivity of 95.0 (X cm) 1.
To understand how the Pt ion implantation/post-annealing
processes result in an enhanced conductivity and EFE properties for Pt&A-UNCD films in a local scale, the local electronic properties of the films were investigated by CITS in
STS mode. Figs. 2(a) and 2(c) show the STM images of
P-UNCD and Pt&A-UNCD films, respectively, while the
corresponding CITS mappings, taken at a sample bias of
3 V, are shown in Figs. 2(b) and 2(d), respectively. Bright
and dark regions in the CITS images are visible with their
shapes having similarity with the shapes of the STM
images.25 The typical grain and grain boundary are marked
as 1 and 2, respectively, in STM image in Fig. 2(a) with
the corresponding marking in the CITS image in Fig. 2(b)
for P-UNCD films. Similarly, the grain and grain boundary
are marked as 3 and 4, respectively, in Fig. 2(c) with the

FIG. 2. STM image of (a) P-UNCD and (c) Pt&A-UNCD films with their
corresponding CITS mapping in (b) and (d), respectively.

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163109-3

Panda et al.

corresponding marking in Fig. 2(d) for Pt&A-UNCD films.

The CITS mapping of P-UNCD films in Fig. 2(b) clearly
shows that few emission sites are located along the diamond
grain boundaries. It is evident that the number density of
emission sites is significantly enhanced in Pt&A-UNCD
films than those of the P-UNCD films such that it looks as if
the whole Pt&A-UNCD films surface are emitting.
To know more precisely how the Pt ion implantation/
post-annealing processes affect the number density of emission sites in a local scale, the high resolution STM (HRSTM)
image of Pt&A-UNCD films along with the corresponding
CITS mapping are taken. Fig. 3(a) shows the HRSTM image
with the corresponding CITS mapping in Fig. 3(b), taken at
the sample bias of 3 V. It is observed that the emission sites
are along the grain boundaries marked as GB1, GB2,
and GB3 in Fig. 3(b), indicating that the grain boundaries
are the prominent emission sites. The corresponding grains
marked as G1, G2, and G3 looks dark in the CITS
image [Fig. 3(b)], indicating lower emission. It is to be noted
that some clusters also emit like the grain boundaries,
marked as 1 and 2 in CITS image in Fig. 3(b) with the
corresponding marking in Fig. 3(a). These high electron
emitting clusters may be the metallic Pt nanoparticles, which
appear on the surface of Pt&A-UNCD films due to the postannealing of the Pt implanted UNCD films.
The emission properties observed by CITS mapping for
Pt&A-UNCD films are further crosschecked by local
current-voltage (I-V) characteristic curves. The local I-V
curves from STS measurements at various sample positions
as on the grains and grain boundaries in HRSTM image are

Appl. Phys. Lett. 105, 163109 (2014)

shown in Fig. 3(c). Ten reproducible I-V curves shown in

open symbols and the average of these curves plotted as solid
symbols corresponding to each emission sites as grain (I),
Pt nanoparticles (II), and grain boundaries (III) of
Pt&A-UNCD films shown in Fig. 3(c) were recorded during
the STS imaging. We observed a significant change in I-V
characteristic curves both at the grain and grain boundaries
for Pt&A-UNCD films. The GBs (Fig. 3(c), curve III) emit
at a lower sample bias compared to the grains (Fig. 3(c),
curve I). Few Pt nanoparticles, marked as 1 and 2 in Fig.
3(a), also emit at a lower sample bias (Fig. 3(c), curve II), in
addition to the grain boundaries.
The normalized conductance (dI/dV)/(I/V) at the grain
and grain boundary for the Pt&A-UNCD films are deduced
from the respective I-V characteristic curves shown in Fig.
3(c) and are plotted in Fig. 3(d). The normalized conductance provides information on the surface local density of
states.26,27 A band gap of about 3.4 eV is calculated on
the UNCD grain from the spectra (I) (Fig. 3(c)) for the
Pt&A-UNCD films, which is smaller than 4.2 eV for nanodiamond crystals that has been reported in literature28 and
also proposed by theoretical calculations.29 Lower bandgap of
3.4 eV could be due to the Pt doping and post-annealing process. From the variation of normalized conductance curves
II and III in Fig. 3(d), the band gap further reduces for the
Pt nanoparticles (marked as 1 and 2) and grain boundaries
(marked as GB1, GB2, and GB3), respectively, shown
in the HRSTM image Fig. 3(b).
TEM examination has been carried out to further examine the actual microstructural evolution induced by the Pt ion

FIG. 3. HRSTM image of (a)

Pt&A-UNCD with the corresponding
CITS in (b). (c) The local I-V characteristics curves at the (I) diamond grain
(marked as G1, G2, and G3 in (a)), (II)
Pt nanoparticles (marked as 1 and 2 in
(a)), and (III) diamond grain boundaries (marked as GB1, GB2, and GB3 in
(a)). Each spectrum shown as dark
thick line in (c) is the average of 10
scanned spectra at the designated
points. (d) Normalized differential
conductance (dI/dV)/(I/V) at the (I)
grain, (II) Pt nanoparticles, and (III)
grain boundaries of Pt&A-UNCD
films.

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Panda et al.

implantation/post-annealing processes. Fig. 4(a) shows the typical bright field image for the Pt&A-UNCD films. Inset in Fig.
4(a) shows the selective area electron diffraction (SAED) pattern which illustrates that, besides the diffraction rings corresponding to the (111), (220), and (311) lattice planes of
diamond, there presents an extra diffraction ring corresponding
to Pt material (designated as (111)Pt), confirming the presence
of Pt nanoparticles on Pt&A-UNCD films. Dark-field images
were taken from a different part of SAED, i.e., from the diffraction spots corresponding to diamond, graphite, and Pt separately and the images were then superimposed to clearly
illustrate the distribution of these phase constituents. Figure
4(b) clearly shows that the Pt-clusters (blue color) were uniformly distributed among the UNCD grains (red color) in
Pt&A-UNCD films; so do the nano-graphitic clusters (green
color). More detailed microstructure of Pt&A-UNCD films
were illustrated by TEM. Fig. 4(c) shows the structure image
for a typical region in Pt&A-UNCD films (Fig. 4(a)). Fourier
transformed diffractogram (FT) image of the entire structure
image (FT0) in Fig. 4(c) shows a spotted diffraction pattern
arranged in ring, suggesting nano-sized nature of the diamond
(D) and platinum (Pt) phases. The donut-shaped diffused diffraction ring located at the center of FT0 image corresponds to
graphitic (G) phase. The existence of diamond (D) phase is

FIG. 4. The (a) bright field with corresponding SAED pattern in inset and
(b) dark field (DF) TEM micrographs of Pt&A-UNCD film. (c) Typical
High resolution TEM structure image of Pt&A-UNCD films. The FT image
corresponding to whole structure image is shown as FT0 and the FT images
of the selected regions as 14 are shown as insets FT1FT4, respectively.
Carbon edge (d) core-loss and (e) plasmon-loss EELS spectra of Pt&AUNCD films.

Appl. Phys. Lett. 105, 163109 (2014)

highlighted by region 1, the platinum (Pt) phase by regions 2

and 3, the graphitic phase by region 4 and are identified by the
FT images FT1, FT2, FT3, and FT4, respectively. Interestingly,
the presence of graphitic phase is closely associated with the
formation of the Pt nanoclusters. On the basis of TEM investigations for the Pt&A-UNCD film, it is noticed that Pt ion implantation/post-annealing process induces the presence of
nanographitic phases. The emitting particulates in locations
1 and 2 observed in Figs. 3(a) and 3(b) are probably the
nanographitic layer encapsulating the Pt-nanoparticles.
To elucidate the localized bonding structure, for better
understanding the genuine mechanism that enhance the EFE
properties for Pt&A-UNCD films, the carbon K-edge electron energy loss spectroscopy (EELS) was examined to
unambiguously distinguish between the different carbon
materials such as diamond, graphite, and a-C.30 Fig. 4(d)
shows core-loss EELS spectrum of Pt&A-UNCD films
indicating a small hump, representing sp2-bonded carbon
(285 eV, p*-band), besides the typical EELS signal of
sp3-bonded carbon, i.e., a sharp peak at 292 eV (r*-band)
and a dip in the vicinity of 302 eV12,31 that indicated clearly
the presence of abundant sp2-bonded in Pt&A-UNCD films.
In contrast, plasmon-loss EELS spectrum of Pt&A-UNCD
shown in Fig. 4(e) reveals that the sp2-bonded carbon contained in these films is graphitic in nature, as it contains a
large diffuse peak near 27 eV.32,33
Apparently, the grain boundary graphitic phases existing
among the diamond grains of the UNCD films create conduction channels for easy transport of electrons and hence
enhanced the electrical conductivity and EFE properties for
Pt&A-UNCD films that is in accord with the literature
reports.12,13,34,35 The electrons can transported easily through
the nanographitic phases to the emitting surface and then emitted to vacuum easily as the diamond surfaces are NEA in
nature.4,5
In summary, we have demonstrated a feasible way of
fabricating conducting UNCD films with enhanced EFE
properties due to Pt ion implantation/post-annealing processes. Significant enhancement in emission site densities are
observed in Pt&A-UNCD films compared to the P-UNCD
films. The high resolution CITS mapping and local IV characteristic curves clearly revealed that the electrons are dominantly emitted from the diamond grain boundaries and Pt
nanoparticles. The formation of nanographitic phases among
the diamond grain boundaries and around the Pt nanoparticles advance the conducting nature of the films by easy
transport of electrons that is possibly the prime reason for
enhanced EFE properties for Pt&A-UNCD films. The superior EFE characteristics of conducting Pt&A-UNCD films
via simple Pt ion implantation/post-annealing may open up a
pathway for the application in high-definition flat panel displays or plasma devices.
The authors would like to acknowledge the financial
support by Japan Society for the Promotion of Science
(JSPS) to carry out this research work.
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