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Correlation between ID⁄IG Ratio from Visible Raman Spectra and sp2/sp3 Ratio
from XPS Spectra of Annealed Hydrogenated DLC Film

Article in MATERIALS TRANSACTIONS · July 2006

DOI: 10.2320/matertrans.47.1847

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Materials Transactions, Vol. 47, No. 7 (2006) pp. 1847 to 1852
#2006 The Japan Institute of Metals EXPRESS REGULAR ARTICLE

Correlation between ID =IG Ratio from Visible Raman Spectra and sp2 /sp3 Ratio
from XPS Spectra of Annealed Hydrogenated DLC Film
F. C. Tai1; * , S. C. Lee1 , C. H. Wei2 and S. L. Tyan3
1
Department of Material Science and Engineering, National Cheng-Kung University, Tainan 701, Taiwan
2
Department of Mechanical Engineering, TATUNG University, Taipei 104, Taiwan
3
Department of Physics, National Cheng-Kung University, Tainan 701, Taiwan

The hydrogened diamond like carbon film (DLCH) with 1 mm thickness is made by hydrocarbon gas ion beam deposition method. The
relationship between ID =IG ratio fitted from visible Raman spectra and sp2 /sp3 ratio done from XPS spectra of DLCH film shows a trend. The
ID =IG ratio of deconvoluted visible Raman spectra shows a correlation with sp2 /sp3 ratio from XPS spectra as annealing temperature increases,
the graphitization and the disorder increase. The ID =IG ratios fitted with two-curve Gaussian functions of Raman spectra tend to be proportional
to sp2 /sp3 ratio fitted with three-curve with 100% Gaussian function of XPS spectra when post annealed treatment is below 400
C and without
severe oxidation. [doi:10.2320/matertrans.47.1847]

(Received March 6, 2006; Accepted May 22, 2006; Published July 15, 2006)
Keywords: hydrogenated diamond like carbon (DLCH) film, Raman spectra, XPS spectra, ID =IG ratio, sp2 /sp3 ratio

1. Introduction
It is well known that there are a lot of analytical techniques
used to quantify the versatile properties of diamond-like
carbon (DLC) film from different manufacturing processes.1)
Among these tools, spectrum shape fitting is a useful method
to show the detail structure of carbon films. There are two
kinds of quantitative indexes that can evaluate DLC’s
characteristics; one is ID =IG ratio which is often used to
evaluate the disorder of carbon networks, ID means the
intensity of decomposed D (disorder) peak due to the A1g D
breathing carbon bonded modes of sp2 disordered carbon
atoms sites as aromatic rings structure, and IG means the
intensity of decomposed G (graphite) peak resulted from the
E2g G stretching carbon bonded mode of all pairs of sp2
disordered atoms as both aromatic and olefinic molecules.
Visible Raman spectroscopy with 488 or 514 nm wavelength
is the most popular tool to measure ID =IG ratio due to the
nondestructive nature and easy operation.2,3) The other index
is sp2 /sp3 ratio which is used to evaluate the graphitization of
carbon networks. In this index sp2 means the intensity of
decomposed sp2 peak with graphite-like property due to
trigonal coordination carbon network and sp3 means the
intensity of decomposed sp3 peak with diamond-like property
due to tetrahedral coordination carbon network. X-ray
photoelectron spectroscopy (XPS) is the better method to
measure sp2 /sp3 ratio compared with Auger electron spec-
troscopy (AES), electron energy loss spectroscopy (EELS),
nuclear magnetic resonance (NMR) due to measuring
superiorities.4–6) In finding the correlation between ID =IG
ratio and sp2 /sp3 ratio of non-hydrogenated Diamond-Like
Carbon film (DLC) film, some studies have used Raman
spectra associated with EELS or XPS.7–12) But for DLCH
film, due to the spectrum of visible Raman contains a much
larger scattering cross section of sp2 than that of sp3 up to 50–
230 times,13) it is very difficult to detect the sp3 content when
the sp3 content in DLCH film is small. As a result, visible
Raman can’t be directly applied to probe sp2 /sp3 ratio. The
*Corresponding author. E-mail: fc.tai@msa.hinet.net
sp2 /sp3 ratio then can be quantified by Tamor’s data fitting
curve of optical Tauc gap energy by calculating the sp3
component measured by EELS or NMR as noted by Ferrari.2)
The purpose of this study is to find out a correlation between
ID =IG ratio by visible Raman and sp2 /sp3 ratio by XPS of
DLCH films under post annealed treatment.
2. Experimental Procedure
DLCH film was performed by direct carbon ion beam
deposition (IBD) method with hydrocarbon gas to deposit on
600 (100)-oriented p-type single-side polished silicon wafer.
The vacuum chamber was installed with four sets of ion beam
sources, when the base pressure reaches the 5  104 Pa with
Ar as purging gas, then the reactive hydrocarbon gas was fed
through the ion source with special Reflector Anode Hot
Wire Filament to accelerate these ionized species until stable
working pressure reached at 0.1 Pa. The DLCH growth
temperature was controlled at 200
C, and the final deposited
thickness was 1.0 mm. The typical hydrogen content of
DLCH films deposited by IBD method ranged from 30 to
40 at%.1) The post annealed temperatures of thermal treat-
ment were set at 300
C, 350
C and 400
C under N2
atmosphere for one hour, respectively.
Raman spectroscope was used to confirm the amorphous
structural characteristic of DLCH film, the Arþ laser wave-
length was 488 nm and the probe aperture was near 10 mm, in
order to avoid local heating accumulation during film
detection, the lower laser power output (14 mW) was used
and substrate holder was controlled at 77 K from liquid N2 ,
there is no visible damage before and after Raman test. The
curve-fitting of raw Raman line was deconvoluted into two-
curve with one linear background normalization. According
to automatic fitting of integrated area it is not necessary to fix
the D and G peak position and full width at half maximum
(FWHM), respectively. XPS tool (Model Escalab 210) used
Al k-alpha radiation (1486.6 eV) and chose polyethylene as
calibration sample (C1s spectrum was set at 284.6 and its sp2
is zero percent). There is no Arþ sputtering as pre-clean
treatment in order to avoid hybridization transformation of
1848 F. C. Tai, S. C. Lee, C. H. Wei and S. L. Tyan

Table 1 XPS C1s spectra deconvolution of carbon films.

2
Material Multi-peaks Fitting function Sp band Sp3 band Sp2 satellite band CO band Sp2 /Sp3 ratio C1s vs. O1s intensity Ref.
X%Gaussian
a-C 2 284.30 285.20 N/A N/A 60/40 N/A 15)
+ Y%Lorentzian
X%Gaussian
a-C 3 284.40 285.20 N/A 286.50 67/33 3.0% O[AT] 16)
+ Y%Lorentzian
80%Gaussian
a-C 3 284.84 285.80 286.85 287.00 67/33 8.0–10.0% O[AT] 17)
+ 20%Lorentzian
a-C 4 100% Gaussian 284.80 285.80 286.90 287.00 80/20 C1s<O1s 18)
80%Gaussian
a-C:H 2 Esp2 Esp2 +0.50 N/A Esp2 +0.50 47/53 C1s>O1s 19)
+ 20%Lorentzian
a-C:H 3 N/A 284.30 285.05 N/A 286.40 20/80 10.0% O[AT] 20)
80%Gaussian
a-C:H 3 Esp3 0.5 variable N/A 3
Esp 0.50 40/60 C1s>O1s 21)
+ 20%Lorentzian
a-C:H 4 N/A 284.50 285.30 286.60 287.70 88/12 N/A 22)
a-C:H:Cr 1 N/A 284.60 N/A N/A 288.60 N/A Air oxidation 23)
X%Gaussian
a-C:H:Ar 3 284.50 285.30 N/A 286.50 26/74 N/A 24)
+ Y%Lorentzian
a-C:H:Si 3 N/A 284.00 284.70 N/A 287.00 N/A 9.2–12.9% O[AT] 25)
a-C:H:N 4 100% Gaussian 284.5 285.50 (C=N) 286.20 (C-N) 287.40 N/A N/A 26)
a-C:H:N 4 100% Gaussian 282.20 284.80 C-N (289.0) 286.50 63/37 N/A 27)
a-C:H:F 4 N/A < 284:9 N/A N/A 287.4 N/A N/A 28)

carbon atom and different sputtering yield during ion

bombardment procedure on top 5 nm depth of near surface
of DLCH film.4,14) XPS was performed to estimate the sp2 /
sp3 area ratio resulting from relative sp2 and sp3 contents of
the DLCH film. The curve-fitting of raw XPS C1s line was
Intensity (a.u.)

also deconvoluted into two-curve, three-curve and four-curve

400°C
types with linear background normalization. All the key 350°C
300°C
parameters were allowed to vary under adopting automatic G
fitting of integrated area method in order to get the
appropriate fitting results, e.g. sp2 , sp3 , sp2 satellite, CO D

(C–O or C=O) peak positions and FWHM, respectively. The as-deposited

raw XPS lines were automatically calculated by 100%
Gaussian function and multi-peaks assignment to get ana-
lytical peak. Table 1 summarizes the XPS C1s spectra
deconvolution of carbon films, including amorphous carbon
film (a-C), a-C:H (DLCH) and a-C:H:X (doping cases), the
different curve fitting methods using 80% up to 100%
Gaussian functions consist of two, three or four deconvoluted
peaks in order to quantitatively evaluate the sp2 /sp3
ratio.15–28) Diez et al. have mentioned that the Gaussian
function could be used to account for the instrumental energy
resolution and chemical disorder, and the Lorentzian function
could be used to measure the life time of photoionzation
process.15)
3. Results and Discussion
3.1 Evaluation of ID =IG ratio by Raman analysis
Figure 1 shows the typical and deconvoluted Raman
spectra of disordered graphite of as-deposited and annealed
DLCH film. In general, two-curve Gaussian function is
simple and sufficient to decompose the single Raman spectra
into two peaks. The deconvoluted D peak means the disorder
carbon bonding centered at around 1350 cm1 and G peak
means the graphite carbon bonding located at around
1580 cm1 .2,29) As increasing the annealed temperature, the
1000 1200 1400 1600
-1
1800 2000
Raman Shift, r / cm
Fig. 1 Raman spectra of as-deposited and annealed DLCH films, the D and
G peaks are deconvoluted by two-Gaussian peaks.
D peak gradually grows and its height is less than that of
G peak until severe annealed treatment under higher temper-
ature, which means the DLCH film becomes less diamond-
like due to annealed treatment. These Raman lineshapes have
a slight skewed potential for D and G peak to shift higher
peak position when DLCH films are annealed from as-
deposited to 400
C state. The variation of both G peak
position, G peak position and ID =IG area ratio are common
criteria for evaluation about post-annealed treatment of
DLCH film. Figure 2 reveals the G peak position and FWHM
of G peak under peak’s integral intensity measured by 100%
Gaussian and two-curve fitting method under as-deposited
and annealed conditions. The result shows the G peak
position shifts from 1555 cm1 (as-deposited) to 1566 cm1
(annealed at 400
C) but FWHM of G peak gradually
decreases from 142 cm1 to 123 cm1 , respectively. This
trend is agreement with the studies of Chiu and Tallant et
 Correlation between ID =IG Ratio from Visible Raman Spectra and sp2 /sp3 Ratio from XPS Spectra of Annealed Hydrogenated DLC Film 1849

150
as-deposited
G Peak FWHM, p / (cm )
-1

140
C1s
130

120

110

Intensity (a.u.)
O1s

100
0 50 100 150 200 250 300 350 400 450 Auger O (KLL)
1600

1580
-1
G Peak Position, p / cm

1560

1540

1520

1500
0 50 100 150 200 250 300 350 400 450
0 200 400 600 800 1000
Annealed Temperature, T / °C
Binding Energy, Ε /eV

Fig. 2 G peak position and FWHM of G peak as a function of annealed

temperature of DLCH films, 25
C sample means the as-deposited state. Fig. 4 Typical survey scan spectrum of DLCH film.

4.0
Uglov et al, a-C film by CAVD method
this work C1s spectra
Chiu et al, Cr-DLCH by CAE method 285.2
3.5 Oral et al, a-C:H film by PECVD method 400°C
Tang et al, DLCH film by MSIBD method 350°C
284.8
300°C
3.0 as-deposited

2.5
Intensity (a.u.)
ID/IG ratio

2.0

1.5

1.0

0.5

0.0
275 280 285 290 295 300
0 50 100 150 200 250 300 350 400 450 500
Binding Energy, Ε /eV
Annealed Temperature, T / °C

Fig. 5 XPS C1s spectra of DLCH films.

Fig. 3 ID =IG ratio as a function of annealed temperature. 25
C samples
mean the as-deposited states.

3.2 Evaluation of sp2 /sp3 ratio by XPS analysis

23,30–36)
al. Figure 3 displays the ID =IG ratio as a function of The XPS C1s and O1s scan spectra of as-deposited of
annealed temperature and compared to other papers.23,31,32,37) DLCH film is shown in Fig. 4. The major characteristic is the
It can be verified that the as-deposited DLCH film contains relative height of C1s peak is higher than O1s peak.
the diamond-like property due to its ID =IG ratio (1.72) is According to the peak area and sensitive factor of carbon
similar to reports from Ma (1.30), Sung (1.70), Sheeja (1.76) (SF is 1.00) and oxygen atom (SF is 2.93), it is easy to obtain
and Zhang (1.80), which are especially characterized on the chemical composition of DLCH films from the measure-
hardness performance.38–41) The ID =IG ratio increases from ment of normalized area. The ratio of oxygen to carbon
1.72 to 2.04 with increasing annealed temperature from as- atomic fraction values for as-deposited, 300
C, 350
C and
deposited to 400
C with one significant variance at 300
C 400
C are 10.9/89.1(0.12), 12.3/87.7(0.14), 14.6/85.6(0.17)
and this means that annealed DLCH starts to increase its and 15.1/84.9(0.18), respectively. These data indicate the
disorder performance at this critical temperature, these values oxygen content will increase with increasing annealed
are consistent with the experimental result by Tallant, Oral temperature even though the thermal treatment is filled with
and Tang et al.30–36) According to these characteristics, the N2 circulation. This content of oxygen is only slightly higher
annealed DLCH film has slight graphitization when heating than previous works20,25) and is assumed to cause no effect on
up to 300
C, this critical temperature is in agreement with the measuring the contents of sp2 and sp3 contents in DLCH film.
study that thermal annealing treatment would lead to lose the Figure 5 shows the XPS C1s spectra of as-deposited and
hydrogen and result in the graphitization conversion for C-C annealed DLCH film. These peaks of lineshapes seem to shift
sp3 bonded carbon to transform to C-C sp2 bonded carbon.33) lower binding energy site from 285.2 eV of as-deposited
On the other hand, 350
C and 400
C post annealed treatment sample to 284.8 eV of annealed one at 400
C with a
result in a more significant change of DLCH films. difference of 0.4 eV and the XPS C1s spectra broadens from
1850 F. C. Tai, S. C. Lee, C. H. Wei and S. L. Tyan

O1s spectra (a)

533 as-deposited
532.2
400°C
350°C
300°C
as-deposited
2
sp

Intensity (a.u.)
Intensity (a.u.)

Fitting not well

3
sp

280 285 290 295

520 525 530 535 540 545 Binding Energy (eV)
Binding Energy, E / eV

Fig. 6 XPS O1s spectra of DLCH films.

(b) as-deposited

FWHM at 1.65 eV of as-deposited sample to 1.78 eV of

annealed one at 400
C with a difference of 0.13 eV. XPS O1s
spectra also shifts from binding energy at 533.0 eV of as- Intensity (a.u.) sp
2

deposited sample to 532.2 eV of annealed one at 400
C with

a difference of 0.8 eV and the XPS O1s spectra broadens
from FWHM at 2.13 eV of as-deposited sample to 2.89 eV of
CO
annealed one at 400
C with a difference of 0.76 eV, as shown sp
3

in Fig. 6, these trends of XPS C1s and O1s spectra are similar
to the findings of the severe oxidation under post annealed at
300
C (noted that at 400
C the Cr-DLCH film is severely 280 285 290 295
damaged and completely disappeared) for 30 minutes under Binding Energy (eV)
air ambient (Chiu et al.23)). Figures 7(a), (b) and (c) show the
deconvolution results of XPS C1s line by using two curve-
fitting, three curve-fitting and four curve-fitting methods with (c)
as-deposited
100% Gaussian function, respectively. The binding energy
assigned to sp2 , sp3 , sp2 satellite and CO part ranges from low
energy site to high energy site. The asymmetric component is sp
2
Intensity (a.u.)

located at the higher binding energy site. By comparing to

Raman spectra, the obvious characteristics of XP1 C1s
spectrum is that the curve is asymmetric and the non- 2
sp satellite
deconvoluted peak position ranges around 285.0 eV with a 3
sp CO
deviation of 0.2 eV where the peaks comes from the C-C, C-
H and C-OH bonds of DLCH film. It is easy to break these
bonds with appropriate thermal energy but it is hard to
separate these relative components.14) Franta et al.42) have
280 285 290 295
proposed optical dispersion model to illustrate the linear Binding Energy (eV)
relation between annealed temperature and sp2 /sp3 ratio of
DLCH deposited by PECVD method. Diaz et al.15) also have Fig. 7 (a) Two-Gaussian peaks fitting deconvolution of XPS C1s spectra of
found the same trend from a-C film by laser evaporation. DLCH films, (b) and (c) are three and four peaks.
From these trends and the fitting accuracy of Fig. 7(a), it is
concluded that the two-curve fitting method is not a suitable
choice in order to separate the sp2 and sp3 contents, as shown XPS measurement results, the three-curve fitting demon-
in Fig. 8. It is noted that the sp2 /sp3 ratio increase from 3.70 strates a better relationship between oxygen content and CO
to 6.25 with increasing annealed temperature from as- content than the four-curve fitting. Finally, it is reasonable to
deposited to 400
C, which means that DLCH film starts determine the relationship between ID =IG ratio and sp2 /sp3
gradual graphitization and the graphite-like part increases ratio (Fig. 10) by combining the Figs. 3 and 8. For DLCH
with increasing temperature under annealed treatment. film when post annealed treatment is under 400
C with slight
Figure 9 shows the XPS O1s spectra of as-deposited and oxidation, the ID =IG ratio could correlate linearly with sp2 /
annealed DLCH film, and there exists a trend that the CO sp3 ratio by adopting the three-cure fitting method with 100%
content increases with oxygen content either by three-curve Gaussian function, and this trend is similar to the findings of
fitting or four-curve fitting method on C1s spectrum. But by Ferrari, Reisel and Zhang et al. by using Raman and
comparison with sp2 /sp3 ratio chart and oxygen content of EELS.2,6,43)
 Correlation between ID =IG Ratio from Visible Raman Spectra and sp2 /sp3 Ratio from XPS Spectra of Annealed Hydrogenated DLC Film 1851

10 4.0
four-curve fitting
9 three-curve fitting
two-curve fitting 3.5 Ferrari et al, a-C:H film by NMR and EELS analysis

8
3.0
7

2.5
6
sp /sp ratio

ID/IG Ratio
3

5 2.0 this work (XPS)

2

4
1.5

3 Zhang et al, a-C and a-C:H film by EELS analysis

1.0 Reisel et al, a-C:H:N by NMR analysis

2

0.5
1

0 0.0
0 100 200 300 400 500 0 1 2 3 4 5 6 7 8 9 10
2 3
Annealed Temperature, Τ / °C sp /sp ratio

Fig. 8 sp2 /sp3 ratio as a function of annealed temperature by multi- Fig. 10 ID =IG ratio as a function of sp2 /sp3 ratio by three-Gaussian peaks
Gaussian peaks fitting deconvolution of XPS C1s of DLCH film. fitting method of XPS C1s of DLCH film.

Acknowledges
40

four-curve fitting The authors thank the assistance from the Cosmovac
three-curve fitting
35 Company for deposition the DLCH film and Dr. C.H. Wu of
Prof. S. L. Tyan Laboratory (Department of Physics, NCKU)
30
for Raman measurement and discussion.
CO percent (%)

25
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4. Conclusions
The hydrogened diamond like carbon film (DLCH) with
1 mm thickness is deposited by direct hydrocarbon gas ion
beam method on silicon wafer. Experimental results show
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necessary to fix the peak position, peak height and FWHM of
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