Pulsed Electron Beam Deposition of

Nanocrystalline Diamond
Redhouane Henda and Omar Alshekhli
Laurentian University

Bharti School of Engineering/Laurentian University

Sudbury, Ontario P3E 2C6

OBJECTIVES

BACKGROUND
! Nanocomposites of NCD consist of nanometer sized diamond grains (crystallites)
surrounded by an amorphous carbon matrix (Figure 1). Diamond grains contain only
sp3 hybridized carbon atoms, while the amorphous carbon phase consists of both sp3
and sp2 hybridized C atoms (and possibly hydrogen). At the interface of these two
phases are grain boundaries (Figure 2) (1-3). The attractive properties of NCD such as
chemical inertness, electronic and mechanical properties, and other characteristics
make NCD an ideal material for many applications.
! Numerous attempts have been made to deposit NCD. These include plasma enhanced
chemical vapor deposition, ion beam deposition, cathodic arc deposition, magnetron
sputtering of carbon targets, and pulsed laser deposition (PLD). It has proven to be
quite challenging to prepare NCD films and optimize their properties to meet certain
requirements of a given application. Therefore, more advanced/novel deposition
techniques need to be assessed for their potential to prepare NCD thin films of various
properties. This study is a contribution towards this concerted research effort.
! Channel-spark pulsed electron beam ablation (PEBA)* is based on the nonequilibrium evaporation (4, 5) of a target [highly order pyrolytic graphite (HOPG), in
this case] through the application of a self-pinched pulsed electron beam (Figure 3).
PEBA has an electric-to-electric energy conversion efficiency of > 30% (5), making it
an effective technique for the preparation of thin films. Many parameters that control
the quality of deposited thin films via PED must be judiciously selected. These include
energy (power) density, electron energy, pulse rate, background gas and other
geometrical features of the chamber.

Figure 1: SEM image of

nanocrystalline diamond (6)

Figure 2: Structure model

for NCD (6)

Figure 3: Simplified
schematics of a PED system

* PEBA is a technology licensed from Forschungszentrum Karlsruhe

EXPERIMENTAL DETAILS
Thin films of nanocrystalline diamond have been prepared from a HOPG target
(HOPG ZYB, Optigraph GmbH, Germany) (Figure 4) under a background of argon
gas. A typical deposition run is shown in Figure 5. The thickness of the resulting thin
films is in the range 50 nm 120 nm (see inset, Figure 9). NCD Films have been
deposited on various substrates of silicon (Figure 6), namely, Si(100) and Si(111), at
two different substrate temperatures, namely, room temperature and 150C (run #
2), and at ablating pulses of 3,000 (runs # 1-3) and 5,000 (run # 4). The films have
been characterized using AFM (Bruker), visible Raman spectroscopy (HORIBA Jobin
Yvon XploRA), and visible reflectance spectroscopy (Semiconfsoft), and SEM (FEI
Quanta 650F, 20 kV, spot size = 3.5).

" Reporting on the potential of PEBA toward the deposition of thin films of nanocrystalline
diamond from a HOPG target.
" Investigation of optimal deposition conditions.
" Characterization and analysis of the deposited films via numerous analytical methods.

RESULTS & DISCUSSION

! Visible Raman spectra (514 nm) of NCD coatings
on Si (100) and Si (111) are shown in Figure 8. The
spectra show five signals (obtained using a Gaussian
deconvolution) at 1150, 1332, 1350, 1480 and
1550 cm!1. The recorded signals are indicative of the
presence of NCD in the films (2). The position of the
G peak has been used to determine sp3 contents in
the deposited films using Yadavs relation (7).

Table 1: The position of G peak and sp3

content

Run Sample
1
2
3
4

Si(100)
Si(111)
Si(100)
Si(100)

G
position
1534
1536
1571
1537

sp3%
47.494
46.516
29.401
46.027

sp3 content = 0.24 - 48.9("G - 0.1580)

Where "G (m-1) represents the value of the G peak
position. Table 1 shows the position of the G peak
and sp3 content in films prepared from all runs. The
sample prepared at 150C (run # 3) contains the
lowest percentage of sp3.
! The morphology of the films as revealed by AFM
analysis, see Figure 10, consists of clusters of
crystallites in the range 50 nm to 1 m. The clusters
grow along a preferential direction. With respect to
grain size criterion, films resulting from runs 1, 2,
and 4, are consistent with the grain size expected for
NCD. The cluster size does not appear to be
uniformly distributed over the surface. AFM image
of run # 3 (150C) does not show well developed
clusters relatively to NCD films obtained at room
temperature. This is consistent with the results
obtained from Raman analysis. AFM images also
show larger size NCD clusters as the number of
electron beam pulses is increased from 3,000 pulses
to 5,000 pulses.

Figure 8: Raman signal for film on Si in

Run 1, 2, 3, and 4

Si(100) - Run1, Ra = 3.06

Si(111) Run2, Ra = 22.2

! SEM images (Figure 11) of films reveal variations

in the morphology of films deposited at RT (run # 1)
and at 150C (run # 3). The former seem to be more
continuous than the latter, in good agreement with
AFM data.

Run Substrate
1
2
3
4

Figure 6:
Silicon (100)
bare substrate

Si(100)
Si(111)
Si(100)
Si(100)

Thickness
(nm)
72.42
55.96
60.22
113.74

Si(100) Run3, Ra = 57.4

Si(100) Run4, Ra = 71.7

Figure 10: AFM of NCD film deposited on

Si in Run 1, 2, 3, and 4

Figure 7: NCD
coating on
Si (100)
Figure 4: HOPG Target Disk (25
mm diameter X 5 mm thickness)

Figure 5: Ablation and plume inside

the deposition chamber

Figure 9: Measured and calculated reflectance data

CONCLUSIONS

Nanocomposites of NCD have been successfully obtained via PEBA under judiciously selected process conditions.
NCD has been identified using visible Raman spectroscopy.
AFM and SEM analyses of NCD films have shown cluster size to vary between 50 nm and up to the micron range.
NCD clusters are better developed at room temperature in terms of their size and structure.
The growth of larger NCD clusters also seems to be favoured by a large number of ablating pulses (thicker films).

Figure 11: SEM images of films on Si at RT

(left) and 150C.

We wish to thank the Canada Foundation for Innovation (CFI)

and the Natural Sciences and Engineering Research Council of
Canada (NSERC) for the financial support.

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