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Optical emission spectroscopy of the

active species in nitrogen plasma
a a a a
A. Qayyum , Shaista Zeb , M. A. Naveed , S. A. Ghauri , A.
b a
Waheed & M. Zakaullah
a
Department of Physics , Quaid-I-Azam University , 45320,
Islamabad, Pakistan
b
Pinstech , PO Box 2151, 44000, Islamabad, Pakistan
Published online: 21 Aug 2006.

To cite this article: A. Qayyum , Shaista Zeb , M. A. Naveed , S. A. Ghauri , A. Waheed & M.
Zakaullah (2006) Optical emission spectroscopy of the active species in nitrogen plasma, Plasma
Devices and Operations, 14:1, 61-70, DOI: 10.1080/10519990500281659

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 Plasma Devices and Operations
Vol. 14, No. 1, March 2006, 61–70

Optical emission spectroscopy of the active

species in nitrogen plasma
A. QAYYUM†, SHAISTA ZEB†, M. A. NAVEED†, S. A. GHAURI†, A. WAHEED‡ and
M. ZAKAULLAH*†
†Department of Physics, Quaid-I-Azam University, 45320 Islamabad, Pakistan
Downloaded by [Aston University] at 14:36 22 April 2014

‡Pinstech, PO Box 2151, 44000 Islamabad, Pakistan

(Received 14 February 2005)

Optical emission spectroscopy is used to study the production of active species in nitrogen plasma
excited by a 50 Hz pulsed-dc power source. The emission intensities of the band heads of the second
positive (λ = 337.1 nm; 0–0) and first negative (λ = 391.4 nm; 0–0) systems are used to investigate
the dependence of their radiative states N2 (C 3 u ) and N+ 2 +
2 (B u ) population density on operating
parameters. The emission intensity of the N+ 2 (B 2  + ) radiative state is used to determine the relative
u
dependence of N+ 2 ion density on operating conditions by considering the fact that, in low-temperature
plasmas, the dominant mechanism of the population of N+ 2 +
2 (B u ) state starts from the ground state
N+2 (X 2  + ) mainly by electron collisions. It is found that the production of these active species has
g
a significant dependence on the discharge parameters and may be optimized under typical operating
conditions.

Keywords: 50 Hz pulsed-dc generated nitrogen plasma; Plasma-induced optical emission spectro-

scopy; Excited-state population density

1. Introduction

Glow discharge plasmas are usually used in an abnormal glow regime for material processing,
because in this operational mode the cathode is fully covered by the glow, which offers the
possibility of uniform surface ion implantation by high-energy ions [1]. The bias applied on
the substrate may be dc or pulsed dc. However, pulsed dc is more favourable, as it gives
rise to the formation of more radicals and prevents transition to an arc [2]. The increased
cathode fall region in the abnormal glow mode generates faster electrons and ions; so the
negative glow region expands and the high-energy ions bombard the cathode [3, 4]. The
substrate, which also serves as a cathode, is bombarded by positive ions coming mainly
from the negative glow region, where they are created by inelastic collisions with high-energy
electrons. Since a pulsed discharge can operate at much higher peak voltages and peak currents

*Corresponding author. Emails: mzakaullah@qau.edu.pk; zaka_qau_pk@yahoo.com

Plasma Devices and Operations

ISSN 1051-9998 print/ISSN 1029-4929 online © 2006 Taylor & Francis
http://www.tandf.co.uk/journals
DOI: 10.1080/10519990500281659
 62 A. Qayyam et al.

for the same average power as a dc glow discharge, higher instantaneous sputtering, ionization
and excitation can be expected, and hence better efficiencies. This is because the basic plasma
phenomena, such as excitation and ionization, are highly nonlinearly dependent on the field
strength [5, 6]. As far as basic plasma processes are concerned, a pulsed glow discharge is
very similar to a dc glow discharge; that is, it can be considered as a short dc glow discharge,
followed by a generally longer afterglow, in which the discharge burns out before the next
pulse starts. During the ion nitriding process, the active species of nitrogen are generated by
an electric discharge and are diffused into the bulk, making the surface hard. The generation
of these active species relies on the ability of the plasma to produce a high concentration of
excited states of the plasma species, which have an energy several electronvolts above their
ground states and can affect the surface and thus deposition chemistry. Further, it is widely
accepted that the nitrogen ions are thermally diffused into the surfaces resulting in a deep (10–
20 µm) nitrided layer [7]. The ion flux to the cathode also deposits energy and momentum
and thus contributes to heating the surface, which facilitate the impingement of the ions on the
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substrate surface. Moreover, ions play an important role in generating the high-energy neutral
molecules and radicals bombarding the substrate, which also deposit energy and facilitate
the diffusion [5, 6, 8]. The most widely used optical method for sensing neutral and ionic
species in reactive plasmas is optical emission spectroscopy (OES) owing to its non-perturbing
nature [9, 10]. The emission intensity of the electronically excited states of plasma species
is proportional to their population density, which is characterized by both the density of the
plasma species involved in the optical emission and the electron energy distribution function
(EEDF). To relate the ground-state population density of plasma species to the excited-state
population density by means of the measured emission intensity of respective spectral lines,
one has to consider the EEDF and the excitation cross-section of the upper levels together
with the concentration of the species [11]. In low-temperature (below 3 eV) nitrogen plasma
the emission intensity of the N+ 2 molecular band allows easy and accurate spectroscopic
measurement of the N+ 2 ion density in nitrogen glow discharges, where the population of
the excited state N+ 2 +
2 (B u ) is mainly due to the direct electron impact excitation from the
+
ground state of the N2 ion instead of electron impact excitation from the ground state of the
N2 molecule [12, 13].
In this paper, plasma OES of active species is carried out to obtain insight into the species
that affect the plasma reactivity and to gain better understanding of the mechanisms leading
to the production of these active species. In particular, the influence of discharge parameters
such as the input power, filling pressure and gas flow rate on the occurrence of these active
species is studied. The main aim of this work is to find the optimum operating conditions for
the production of these active species for the desired treatment of the samples in a simple and
cost-effective manner.
Section 2 describes the experimental set-up together with the optical diagnostics whereas
different population mechanisms of N2 and N+ 2 radiative states and their dependence on
discharge parameters are presented in section 3. The procedure for the determination of the
relative N+2 ion density is described in section 4 whereas results and concluding remarks are
summarized in sections 5 and 6, respectively.

2. Experimental details

The experiment is carried out using nitrogen as the working gas, and nitrogen plasma is
generated in an abnormal glow regime. The discharge is sustained with 50 Hz pulsed-dc power
 Active species in nitrogen plasma 63

in a parallel plate configuration of electrodes with a diameter of 7.5 cm and a spacing of 6.0 cm
housed in a cylindrical stainless steel vacuum chamber of 40 cm diameter and height. The side
and back of the electrodes are covered with ceramic casing to prevent additional discharge.
The power is applied to the top electrode through the inductive load, which limits the current
during the discharge. The bottom electrode is grounded. The experimental set-up is illustrated
in figure 1. Prior to feeding the nitrogen gas, the chamber is evacuated down to 10−5 mbar
using a rotary vane pump and an oil diffusion pump. The flow of nitrogen gas is monitored
with mass flow meters whereas the pressure in the chamber is recorded by using a capsule-type
dial gauge. Plasma-induced OES is carried out using a computer-controlled system consisting
of a McPherson 2061 monochromator having 1200 grooves mm−1 and a spectral resolution
of 0.01 nm coupled with a side window photomultiplier tube (PMT-9781B) and autoranging
picoammeter (Keithley 485). The system is calibrated using a mercury lamp. The emission
spectra (300 – 600 nm) are recorded as a function of the electrical power (200 –320 W), filling
pressure (5–9 mbar) and gas flow rate (50 –300 sccm) by keeping the corresponding discharge
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parameters constant. Figure 2 shows the spectral lines of the first negative band head (λ =
391.4 nm; 0–0) corresponding to the electronic transition from the ground vibrational level
of the B 2 u+ state to the ground vibrational level of the X 2 g+ state and the second positive
band head (λ = 337.1 nm; 0–0) corresponding to the electronic transition from the ground-
state vibrational level of the C 3 u state to the ground-state vibrational level of the B 3 g
state. The spectrum is recorded at a filling pressure of 5 mbar and input power of 280 W.

AC

Diode Chain

Nitrogen Gas

Capsule
Type Gauge

Optical Window
View Window
Plasma
PMT Valve

Main Chamber

Autoranging
Pico-ammeter

Computer
To vacuum
pump

Figure 1. Schematic illustration of the experimental set-up: PMT, photomultiplier tube.

 64 A. Qayyam et al.

1.20x10-3

1.05x10-3

Emission intensity (a.u.)

9.00x10-4 N2 [B Σ u
+ 2 +
X Σg (0-0)]
2 +
N2[C Π u B Πg(0-0)]
3 3

-4
7.50x10

-4
6.00x10

-4
4.50x10

3.00x10-4

1.50x10-4
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0.00
330 340 350 360 370 380 390 400
Wavelength (nm)
Figure 2. Emission spectrum recorded at a filling pressure of 5 mbar and an input power of 280 W (a.u., arbitrary
units). The first negative band head (λ = 391.4 nm; 0–0) and the second positive band head (λ = 337.1 nm; 0–0) are
identified and labelled in the spectrum.

3. Emission intensity and population of upper states

In nitrogen plasma the population of the N2 (C 3 u ) excited electronic state is mainly caused
by the direct electron impact excitation (having energies above the excitation threshold) from
the ground state of N2 (X 1g+ ) [14, 15]:

N2 (X 1g+ )ν=0 + e −→ N2 (C 3u )ν  =0 + e (E > 11.1 eV).

The subsequent radiative decays emit characteristic photons of the second positive band
head (0–0) having a wavelength of 337.1 nm:

N2 (C 3u )ν  =0 −→ N2 (B 3g )ν  =0 + hν.

Consequently the emission intensity of the second positive band head (0–0) is proportional
to the population density of the N2 (C 3 u ) state [12–15]. Explicitly the relation is

I (337.1 nm) ∝ Nu ,

where I(337.1 nm) is the emission intensity of second positive band head and Nu is the popu-
lation density of the N2 (C 3 u ) state. The measurement of the emission intensity of this band
head provides quantitative knowledge of the N2 (C 3 u ) state population density.
The interpretation of the spectral intensity of the first negative band head (0–0) deserves
special discussion. The N+ 2 +
2 (B u ) excited state can be populated either by direct electron
impact excitation from the ground state of the molecule N2 (X 1g+ ) via [14–16]

N2 (X 1g+ )ν=0 + e −→ N2+ (B 2u+ )ν  =0 + 2e (E > 18.7 eV)

 Active species in nitrogen plasma 65

or stepwise via electron impact ionization of the N2 molecule and then subsequent electron
impact excitation of the molecular ion:

N2 (X 1g+ )ν=0 + e −→ N2+ (X 2g+ )ν  =0 + 2e (E > 15.57 eV),

N2+ (X 2g+ )ν=0 + e −→ N2+ (B 2u+ )ν  =0 + e.

The subsequent radiative decays emit characteristic photons of the first negative band head
having a wavelength of 391.4 nm:

N2+ (B 2u+ )ν  =0 −→ N2+ (X 2g+ )ν=0 + hν.

Again the emission intensity of the first negative band head (0–0) is proportional to the
population of the N+ 2 +
2 (B u ) state [12].
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4. Relative dependence of ion density [N+2 ]

The band head intensity of the transition 0–0 (λ = 391.4 nm) belonging to the first negative
system gives the N+ 2 ion density as a function of operating parameters [12]. The emission
intensity of this band head is proportional to the population of the N+ 2 +
2 (B u ) state [11, 12].
Explicitly the relation is
I (391.4 nm) ∝ Nu ,

where I(391.4 nm) is the emission intensity of first negative band head (0–0) and Nu is the
population of the N+ 2 +
2 (B u ) state. For low-temperature plasmas (below 3 eV) the dominant
mechanism of the population of N+ 2 + + 2 +
2 (B u ) state starts from the ground state N2 (X g )
+ 2 +
mainly produced by electron collisions on N2 (X g ) ions and the excitation rate coefficients
depend very little on the shape of the EEDF [12]. In contrast, excitation from neutral nitrogen
is very sensitive to the high-energy tail owing to the high excitation threshold of about 18 eV
and is much suppressed in low-temperature plasmas. This fact provides the basis for the
measurements of ground-state ion density [N+ + 2 +
2 ] [12]. The population density of N2 (B u )
state is [11–13]
N2+ (B 2u+ ) ≈ kne [N2+ (X 2g+ )].

Since N+
2 (X) ∝ ne , therefore

N2+ (B 2u+ ) ≈ k[N2+ (X 2g+ )]2 .

where k (=10−14 m3 s−1 ) is the N+ +

2 (X) → N2 (B) excitation rate coefficient and is very insen-
sitive to the shape of the EEDF for low-temperature plasmas [12]. Therefore the emission
intensity of the first negative band head should be proportional to the square of the ground-state
ion density [N+ 2 ]:

I(391.4 nm) ≈ k[N2+ ]2 ,

I(391.4 nm) ∝ [N2+ ]2 ,

where [N+
2 ] is the ground-state population density of the nitrogen molecular ion.
 66 A. Qayyam et al.

5. Results and discussion

As stated earlier, the population of the excited states involved in the optical emission is pro-
portional to the electron density whose energy is greater than the excitation threshold and the
concentration of the species. Consequently, the emission intensities of N2 (C 3 u ) and N+ 2 (B
2 +
u ) excited states give their population densities [5, 6]. The results illustrated in figure 3(a)
predict that the emission intensity of the N+ 2 +
2 (B u ) state increases more rapidly than the
3
emission of the N2 (C u ) state with increasing input power up to 280 W and then decreases,
which may be explained as follows. With increase in the input power the energy of secondary
electrons ejected from the cathode owing to the bombardment of positive ions increases and
the excitation cross-section of the N2 (C 3 u ) state decreases with increase in the electron’s
energy. Since the threshold excitation energy of the N2 (C 3 u ) state is 11.1 eV and the thres-
hold ionization energy of N2 is 15.57 eV, which is more sensitive to high-energy electrons than
the excitation of the N2 (C 3 u ) state. Therefore increased N+ 2 +
2 (B u ) emission compared with
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3
N2 (C u ) emission may be explained by the increasing trend of ionization of N2 molecules
into N+2 ions with increase in power. This fact also suggests the expansion of high-energy tail
of the EEDF with increase in input power. The reduction in emission intensities above 280 W
power is due to the escape of high-energy electrons to the wall, which initiates discharge with
the walls of the chamber and lowers the electron energy of the bulk plasma. To avoid this
additional discharge with the wall of the chamber the input power in this system must be kept
below 280 W for a filling pressure of 5 mbar.
The decrease in the emissions of the N2 (C 3 u ) and N+ 2 +
2 (B u ) states with filling pressure
as shown in figure 3(b) indicates the decreased population density of these excited states.
The emission intensity of N+ 2 +
2 (B u ) decreases more rapidly than does that of the N2 (C u )
3

state. This fact may be explained as follows. When pressure in the chamber increases, it causes
an increase in the number of collisions between the electrons and the other plasma species.
As a result the energy transferred from the electrons to the plasma species increases, causing
an increase in the plasma temperature by lowering the electron temperature. So the tail of
the EEDF shifts to lower energies and the number of electrons having an energy above the
threshold excitation energy responsible for the optical emission is reduced. Since the N+ 2 (B
2 +
u ) emission is more sensitive to high-energy electrons than is the N2 (C 3 u ) emission, the
population of the N+ 2 +
2 (B u ) state is affected more significantly than the population of the
3
N2 (C u ) state.
Figure 3(c) depicts the influence of gas flow rate on the emission intensities of the N2 (C
3
u ) and N+ 2 +
2 (B u ) states and shows that the emission intensities of both states slightly
increases with increasing flow rates up to 200 sccm and then decreases in a similar manner.
This fact may be explained as follows. The bombardment of positive ions and other high-energy
plasma species not only releases secondary electrons but also causes sputtering. The atoms of
the cathode material arrive in the glow discharge and are subjected to collisions with electrons
and other plasma species. The excitation and ionization cross-section of metal atoms is higher
for low-energy electrons owing to the lower excitation and ionization threshold energies of
metal atoms compared with the plasma species [6]. Because of excitation and ionization
collisions the electrons are cooled, thereby affecting the emission of the N2 (C 3 u ) and N+ 2 (B
2 +
u ) states. Therefore, the removal of these impurity atoms due to a flow of gas of up to
200 sccm is helpful in raising the energy of electrons. At higher gas flow rates the contribution
of fresh gas injected into the chamber becomes dominant in lowering the electron temperature
compared with raising the electron temperature owing to the removal of impurity atoms.
When fresh gas is injected into the chamber, the particles of the gas having lower energy make
collisions with the high-energy electrons and reduce their energies. Furthermore, at higher
 Active species in nitrogen plasma 67
Downloaded by [Aston University] at 14:36 22 April 2014

Figure 3. Dependence of the spectral intensity of the first negative band head (λ = 391.4 nm; 0–0) and the
second positive band head (λ = 337.1 nm; 0–0) of N+ 2 and N2 molecular systems on (a) the input power, (b) the
filling pressure and (c) the gas flow rate (a.u., arbitrary units).
 68 A. Qayyam et al.

(a) 0.080
Filling pressure = 5 mbar
Flow rate = 50 SCCM
0.072

Emission intensity (a.u.)

0.064
+
[N 2 ] Ion density
0.056

0.048

0.040

0.032

0.024
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240 260 280 300 320

Input power (watts)
(b)
0.080
Input power = 300 watts
0.072 Flow rate = 50 SCCM
Emission intensity (a.u.)

0.064

0.056 +
[N 2 ] Ion density

0.048

0.040

0.032

0.024

4 5 6 7 8
Filling pressure (mbar)
(c)
0.096
Input power = 300 watts
Filling pressure = 5 mbar
0.088
Emission intensity (a.u.)

0.080

0.072

0.064 +
[N 2 ] Ion density

0.056

0.048

0.040
50 100 150 200 250 300
Gas flow rate (SCCM)
Figure 4. Relative dependence of the molecular ion density [N+
2 ] on (a) the input power, (b) the filling pressure
and (c) the gas flow rate (a.u., arbitrary units).
 Active species in nitrogen plasma 69

flow rates, the high-energy electrons, which leave the chamber together with the gas particles
via the outlet valve, also may result in a reduction in the electron’s energy in the bulk plasma.
The band head intensity of the transition 0–0 (λ = 391.4 nm) belonging to the first negative
system is used to determine the functional dependence of the molecular ion density [N+ 2 ] on
the operating parameters, and the results are presented in figure 4. The relative dependence
molecular ion density [N+ 2 ] is monitored by taking into account the fact that, in low-temperature
plasmas (below 3 eV), the dominant mechanism of the population of the N+ 2 +
2 (B u ) state starts
+ 2 +
from the ground state N2 (X g ) mainly produced by electron impact and the excitation rate
coefficients depend very little on the shape of the EEDF [12]. The molecular ion density,
which is an important parameter of the nitrogen plasma, deposits energy and momentum and
thus contributes to self-discharge heating of the surface, facilitating the thermal diffusion of
nitrogen. It is obvious from the results that the ion density has a significant dependence on the
operating parameters, and the ion flux to the substrate can be maximized by the appropriate
selection of the abnormal glow conditions.
Downloaded by [Aston University] at 14:36 22 April 2014

6. Conclusions

Plasma-induced optical emission has been carried out in an abnormal glow regime to optimize
the plasma generation process for production of N+ 2 ions mainly responsible for surface ion
nitriding of materials by cathodic bombardment. The emission intensities of the band heads of
the first negative system (λ = 391.4 nm; 0–0) and the second positive system (λ = 337.1 nm;
0–0) of N2 have been measured as functions of the operating parameters to determine the
functional dependence of the N2 (C 3 u ) and N+ 2 +
2 (B u ) excited states, which have energies
several electronvolts above their ground states and thus can affect the deposition chemistry. The
emission intensity of the N+ 2 +
2 (B u ) excited state is used to determine the relative ion density
+
[N2 ] by considering the fact that, in low-temperature plasmas (below 3 eV), the dominant
mechanism of the population of the N+ 2 + + 2 +
2 (B u ) state starts from the ground state N2 (X g )
mainly produced by electron collisions on N+ 2 +
2 (X g ) ions and the excitation rate coefficients
depend very little on the shape of the EEDF [12]. The results suggest that the N+ 2 ion flux to
the substrate has a significant dependence on the operating parameters and may be optimized
under typical discharge conditions.

Acknowledgements

The work was partially supported by a Ministry of Science and Technology Grant, the
Pakistan Science Foundation project PSF/R&D/C-QU/Phys. (199), the ICSC World Labora-
tory project E-13 CHEPCI Islamabad, a Quaid-I-Azam University Research Grant and the
Higher Education Commission Research Project for Plasma Physics.

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