Silicon (2021) 13:3229–3237

https://doi.org/10.1007/s12633-020-00676-y

ORIGINAL PAPER

Pulsed Laser Ablation of Tin Oxide Nanoparticles in Liquid

for Optoelectronic Devices
Raid A. Ismail 1 & Sule Erten-Ela 2 & Abdulrahman K. Ali 1,2 & Cagdas Yavuz 2 & Khaleel I. Hassoon 1

Received: 29 June 2020 / Accepted: 26 August 2020 / Published online: 1 September 2020
# Springer Nature B.V. 2020

Abstract
Laser ablation of tin oxide (SnO2) nanoparticles (NPs) was carried out by irradiation of tin target in methanol and aqueous NaCl
solutions with nanosecond laser pulses. X-ray diffraction (XRD) studies show that the synthesized nanoparticles are polycrys-
talline tin oxide with tetragonal phase. Scanning electron microscope (SEM) and transmission electron microscope (TEM) were
used for characterization of the shape, particle size and particle distribution of tin oxide nanoparticles. SEM results reveal that the
synthesized NPs have spherical shape and the presence of agglomerated NPs was observed. TEM investigation confirms that the
average particle size of SnO2 synthesized in methanol was 40 nm and in NaCl solution was around 25 nm. The optical energy gap
of SnO2 NPs prepared in methanol and NaCl solutions were 3.8 eV and 3.95 eV, respectively. Energy dispersive X-ray (EDX)
confirms the formation of SnO2 NPs. The parameters of n-SnO2NPs/p-Si heterojunction photodetectors, namely, dark and
illuminated current-voltage characteristics, photovoltaic properties, spectral responsivity and specific detectivity were measured.
The responsivity of the photodetector prepared in NaCl solution was 0.53A/W at 410 nm, while the responsivity of photodetector
prepared in methanol was 0.43A/W at 410 nm.

Keywords Laser ablation . Tin oxide . Nanoparticles . Methanol . NaCl . Photodetector

1 Introduction synthesize SnO2 nanoparticles like spray pyrolysis, hydrother-

Tin oxide is non-toxic and inexpensive semiconducting mate-
rial [1–3]. It considers a promising material for many potential
applications due to its high electrical conductivity and its good
optical transparency in the visible region [4]. SnO2 is an n-
type semiconductor with direct optical energy gap of 3.6 eV at
room temperature. Nanostructured SnO2 has paying attention
due to its size-depended properties [5]. There are many mor-
phologies for synthesized nanostructured SnO2 such as nano-
wires, nanoparticles, nanotubes and nanorods [6].SnO2 used
widely for electrodes, solar cells, gas sensors, rechargeable
lithium batteries, photodetectors, photocatalyst, energy stor-
age, and medicine. Many methods were employed to
* Raid A. Ismail
raidismail@yahoo.com
1
Applied Sciences Department, University of Technology,
Baghdad, Iraq
2
Institute of Solar Energy, Ege University, 35100 Izmir, Turkey
mal, magnetron sputtering, sonochemical, solvothermal, sol-
gel, microwave, co-precipitation, and laser ablation in liquid
[7–11]. The particle size distribution and morphology of SnO2
nanoparticles were found to be depended on the preparation
technique. Laser ablation in liquid (LAL) technique has con-
firmed itself as one of the most powerful physical methods
used for nanofabrication. The advantages of this technique
over the other chemical methods is simple, inexpensive, no
vacuum neede, the high purity of produced colloids NPs, good
control of particle size, narrow particle size distribution, many
morphologies can be obtained, and the strong optical confine-
ment [12,13]. It has been shown that the optical properties of
nanoparticles prepared by laser ablation technique are
depended on the laser fluence, laser wavelength, pulse width,
repletion frequency, and ablated medium [14]. Few data have
been published on the laser ablation of tin oxide in liquid. Usui
et al. [15] prepared tin oxide nanoparticles by laser- fragmen-
tation of ITO target in water. Sankar et al. [16] study the effect
of ablation time and laser fluence on the properties of SnO2
nanoparticles synthesized by laser ablation of tin target in
deionized water. Liu et al. [17] demonstrated laser-induced
photochemical synthesis of SnO2 nanotubes and they showed
3230 Silicon (2021) 13:3229–3237

that the nanotube length can be manipulated by laser

parameters.The structural properties of SnO2 nanoparticles
have been reported extensively. Dhinakar et al. studied the
structural properties of SnO2 nanoparticles prepared by micro-
wave assisted chemical route method [18]. They showed that
the nanoparticles have tetragonal phase and the crystallinity of
SnO2 nanoparticles improved after annealing at T = 550 °C
for 1 h. Chen et al. showed that the tin oxide nanoparticles
prepared by thermal oxidation of anhydrous stannic chloride
(SnCl4) in a propane/air turbulent flame have tetragonal struc-
ture [19]. Salah et al. reported on the production of ultrafine
pure and Mn-doped SnO2 nanoparticles using the microwave
technique and they found that the synthesized SnO2 nanopar- Fig. 1 Schematic diagram of pulsed laser ablation in liquid system
ticles are crystalline in nature with tetragonal phase and the
crystallite size was 7 nm [20]. Herein, tin oxide nanoparticles morphology and particle size nanoparticles. The optical prop-
were prepared by laser ablation of Sn target in methanol and erties of colloidal SnO2 NPs solution was investigated at room
NaCl solutions without using catalyst in order to fabricate temperature by UV-Vis spectrophotometer (Type Metratech).
SnO2NPs/p-Si photodetector. The figures of merit of the n- To fabricate SnO2NPs/Si photodetector, a thin layer of
SnO2NPs/p-Si photodetector were investigated as a function SnO2 was deposited on the mirror-like p-type silicon substrate
of solution type. by dipping the silicon substrates with 0.8cm2 area and electri-
cal resistivity of 1-3Ωcm in two separate vessels containing
colloidal SnO2 nanoparticles. Figure 2 After the dipping of the
2 Experimental silicon substrates, a tihn layer of SnO2 film is deposited on the
silicon surface. Figure 3 shows the SEM images of nanostruc-
To synthesis SnO2 nanoparticles, a tin target of purity of tured SnO2 film deposited on the silicon surface. The back
99.9%, 5 mm thick and area of 1cm2 (provided from Ege side of silicon substrate and their margins were covered with
Asal Metal Tic) was located on the bottom of glass vessel wax in order to prevent the deposition of the SnO2 film.
filled with methanol (provided from BDH) and irradiated with After deposition of the film, the wax was removed and a
laser pulses. The second laser ablation is carried out by irra- thin film of Al was deposited on the back side of the silicon
diating of tin target positioned in 3 mM of aqueous NaCl substrate and SnO2 film by thermal evaporation tehnique
solution. The Sn target was irradiated vertically by second through mask to perform the ohmic contacts as shown in
harmonic generation SHG of Q-switched Nd:YAG laser Fig. 4. The photosensitive area of the photodetector was 1cm2.
(Huafei) operating at repetation frequency of 10 Hz with The current-voltage characteristics of SnO2NPs/p-Si pho-
7 ns pulse duration. We have selected SHG laser pulses due todetector at dark and illumination conditions were measured
to the high absorption coefficient (α) of Sn for 532 nm wave- at room temperature using regulated DC digital power supply,
length and hence the absorption depth (α−1) is small which is electrometer and halogen lamp. A calibrated Jobin-Yvon
usefull for production of small colloidal particles. The laser
was focused on the target with spot size of 0.5 mm (measured
by using carbon paper) using a lens with of focal length of
7 cm. The vessel has facility to rotate continuously during
ablation process to minimize the particle agglomeration.
Laser fluence of around 12 J/cm2/pulse was used for ablation
for two ablation processes after taking into account the trans-
mission of the methanol and NaCl solution to 532 nm wave-
length. The laser energy was measured using calibrated Joule
meter (Gentec). Figure 1 shows the schematic diagram of laser
ablation used in this study.
The structural properties of the SnO2 nanoparticles were
investigated using x-ray diffractometer (Rigaku Smartlab) by
adding drops of SnO2 nanoparticles on glass substrate.
Transmission electron microscope TEM (type CM10
PW6020 Philips-Germany) and scanning electron microscope Fig. 2 Photographs of fresh colloidal SnO2 NPs ablated in methanol (a)
SEM (Zeiss Supra 55) were used to investigate the and NaCl solutions (b)
Silicon (2021) 13:3229–3237 3231

Fig. 3 SEM images of a b

nanostructured SnO2 layer
deposited on silicon prepared (a)
methanol and (b) NaCl solution

monochromator was used to measure the spectral responsivity
of the photodetector in the spectral region 300-1000 nm.
3 Results and Discussion
NaCl solution can be attributed to the larger pH of NaCl so-
lution compared to that of prepared in methanol.
The SEM images of SnO2 NPs prepared in methanol and
NaCl solutions are shown in Fig. 6. The SEM image of SnO2
NPs prepared in methanol shows the formation of spherical

Figure 5 shows the XRD patterns of SnO2 NPs prepared at by

laser ablation in methanol and NaCl solutions. The XRD of
SnO2 prepared in methanol shows the presence of five diffrac-
tions peaks located at 2θ = 32°, 45°, 62, 64°, 73° and 79°
corresponding to (110), (111), (112), (301) and (320) plane,
respectively. These peaks could be indexed to tetragonal poly-
crystalline SnO2 according to JCPDs# 41–1445 [21]. A dif-
fraction peak at 2θ = 31° corresponding to (110) plane also
was observed which is belonged to tetragonal SnO according
to JCPDs# 006–0395 [22]. Another peak was observed at
43.5° which indexed to Sn element. The presence of SnO
can be ascribed to the formation of incomplete tin oxidation
and due to tin vacancy. The appearance of Sn peak in XRD
pattern is due to the laser fragmentation of tin nanoparticles.
The XRD of SnO2 NPs prepared in NaCl solution exhibits
peaks located at 2θ = 27°, 32°, 39°, 45°, 48°, 51°, 55°, 58°,
63°, 64°, 65.5°, 73°, and 79° corresponding to (110), (101),
(200), (111), (211), (220), (002), (310), (112), (301), (202)
and (320) plane, respectively. All these observed peaks are
indexed to the tetragonal polycrystalline SnO2 and the addi-
tional two peaks observed at 31° and 43.5° are related to the
tetragonal SnO and Sn element, respectively. The existence of
new XRD SnO2 peaks and SnO peaks for sample prepared in

Light

Fig. 4 Architecture and electrical configuration of SnO2NPs/p-Si HJ Fig. 5 XRD patterns of SnO2 NPs formed in (a) methanol and (b) NaCl
photodetector solution
3232
a NaCl solutions are shown in Fig. 8. The nanoparticles synthe-
b

Agglomerated NPs
Fig. 6 SEM images of SnO2 NPs synthesized in (a) methanol and (b)
NaCl solution. Inset is high magnification SEM images
nanoparticles with different sizes and the average particle size
was 65 nm and some large particles were also observed due to
the particles agglomeration. The agglomeration can be as-
cribed to the high surface energy of the nanoparticles and to
the Van der waals force.
Similar morphology for SnO2 NPs prepared in NaCl solu-
tion was obtained with average particle size of 45 nm. It is
observed that the concentration of the nanoparticles prepared
in NaCl solution was higher than of that prepared in methanol.
On the other hand, the particles agglomeration and aggrega-
tion were found to be reduced in the case of using NaCl solu-
tion due to the presence of Cl- ions indicate an increase in the
efficiency of the nanoparticles formation [23]. The EDX spec-
tra and analysis of SnO2 NPs prepared in methanol and NaCl
solution are illustrated in Fig. 7 which shows the presence of
peaks related to tin and oxygen elements. The other peaks are
belonged to the substrate.
The [Sn]/[O] weight ratio of the nanoparticles prepared in
methanol and NaCl solutions were 1.03 and 1.2, respectively,
indicating the formation of off-small stoichiometric SnO2
nanoparticles.The concentration of SnO2 nanoparticles was es-
timated using atomic absorption spectroscopy AAS (model
phonex-986 AA, U.K.) and was about 6 μg/ml in methanol
and 9 μg/ml in NaCl solution. The absorption spectra, in the
UV-Vis, of colloidal solutions of SnO2 NPs in methanol and
Silicon (2021) 13:3229–3237
sized in different liquid media exhibits significant absorption
variation in the visible region under the same ablation condition.
As shown, the absorbance of the two solutions decreases
abruptly after 300 nm and then tends to saturate after 350 nm.
A small shoulder at 375 nm was observed in absorption spec-
trum of the nanoparticles prepared in NaCl solution indicates
formation of small size particles. The optical absorbance of
SnO2 NPs prepared in NaCl solution was higher than that of
SnO2 NPs ablated in methanol due to the higher concentration
of nanoparticles and smaller particle size. The optical band gap
Eg of SnO2 NPs was estimated by using Tauc relationship [24]
n
ðαhν Þ ¼ A hν−E g ……… ð1Þ
Where α is the absorption coefficient and hν is the photon
energy. Figure 9 show the (αhν)2 versus photon energy plot
of SnO2 NPs ablated in methanol and NaCl solutions. The
extrapolation of the linear part of the curve to the photon energy
axis gives the value of the optical energy gap [25].The SnO2
NPs ablated in NaCl solution has band gap of 3.95 eV, while
the energy gap of SnO2 ablated in methanol was 3.8 eV. This
difference in the value of the energy gap can be attributed to the
fact that the SnO2 ablated in NaCl and methanol solutions have
different particles size and this will be discuss in detail with
TEM investigation.
The values of optical band gap of synthesized SnO2 NPs
were larger than that of bulk SnO2 (3.6 eV) due to the quan-
tum size effect [26]. The TEM images of SnO2 particles syn-
thesized in methanol and NaCl solutions are displayed in Fig.
10. It is clearly observed that the particles prepared in metha-
nol have different sizes ranged from 20 nm to 100 nm with
average size of 40 nm and some of these particles have spher-
ical shape and the others have irregular shape. This effect can
be attributed to the agglomeration effect accompanied the la-
ser ablation process which leads to the formation of coarser
particles and this result is in good agreement with published
results [27]. TEM image of SnO2 NPs synthesized in NaCl
solution have spherical particles with average size of 25 nm
and agglomerated and aggregated particles have been also
observed. The SnO2 particle size distribution histogram was
determined using software supported TEM analysis as shown
in the inset of Fig. 10. It is a Gaussian type with full width at
half maximum FWHM of 20 nm for particles ablated in meth-
anol and the particles ablated in NaCl solution has Gaussian
distribution with full width of 40 nm.
Figure 11 shows the dark current-voltage characteristics of
SnO2NPs/p-Si heterojunction. A rectifying properties have
been observed (diode-like properties). The rectification factor
was calculated and found to be 175 and 135 for heterojunction
prepared in methanol and NaCl solution, respectively. The
forward current increases with bias voltage and the turn-on
voltage was 1.7 V for heterojunction prepared at methanol
Silicon (2021) 13:3229–3237 3233

Fig. 7 EDX spectra of SnO2 NPs a

prepared in (a) methanol and (b)
NaCl solution

Counts

keV
b
Counts

keV

and 1.4 V for heterojunction prepared in NaCl solution. This
could be due to the high resistivity of SnO2 NPs prepared at
methanol compared to that of SnO2 NPs synthesized in NaCl
solution. The ideality factor β of the heterojunction was de-
termined from diode eq. [28]
qV
I ¼ I o e βKT
Where K is the Boltzmann constant, q is the electron charge
and Io is the reverse saturation current. The saturation current
has been determined from lnIf versus Vf plot (Fig. 12), where
2.5
If is the forward current and Vf is the forward voltage. After
substituting all the constants and Is in Eq. 2, the ideality factor
of the heterojunction prepared in methanol and NaCl solution
were 3.8 and 2.1, respectively. The large value of the ideality
factor of the heterojunction indicates deviation from the ideal
diode due to the surface states [29,30].
ð2Þ The using thermionic emission of current-voltage charac-
teristics of SnO NPs/Si (p-n) heterojunction (region 1), the
barrier height Φ can be given by [31]
5
4.5
4 Methanol solution

3.5 NaCl solution

(αhν) 2(eV/cm)2

methanol
2
3
NaCl solution
2.5
Absorbance

1.5
2
1.5
1
1

0.5
0.5
0
0
1.5 1.9 2.3 2.7 3.1 3.5 3.9 4.3
300 350 400 450 500 550 600 650 700 Photon energy (eV)
Wavelength (nm)
Fig. 9 (αhν)2 versus photon energy of SnO2 NPs synthesized in
Fig. 8 Absorbance of SnO2 NPs ablated in methanol and NaCl solution methanol and NaCl solution
3234 Silicon (2021) 13:3229–3237

Fig. 10 TEM images of SnO2

NPs ablated in methanol (left) and
NaCl solution (right). Inset is the
particle size distribution

KT AA* T 2 NaCl solution and to the decreasing of the particles agglomer-

Φ¼ ln
q IO
Where A is the area of the heterojunction and A* is the
Richardson constant. The barrier height of the SnO2/Si
heterojunctions prepared in methanol and NaCl solution were
0.68 and 0.78 eV, respectively. Table 1 lists the electrical
properties of n-SnO2/p-Si heterojunctions prepared in metha-
nol and NaCl solution.
The illuminated I-V characteristics of the heterojunctions are
illustrated in Fig. 13. The photocurrent is generated after illu-
minated the photodetector with white light. The light absorption
results in the production of e-h pair which increases the current
of the photodetector. The photocurrent of the heterojunction
prepared in NaCl solution is larger than that of the
heterojunction prepared in methanol solution. This can be as-
cribed to the large surface area of the photodetector prepared in
ð3Þ
ation. The presence of Cl− ions prevents the aggregation and
agglomeration of the nanoparticles as well as leads to the for-
mation of smaller particle size (large surface area). The on/off
ratio was estimated and found to be around 300 and 450 for
photodetector prepared in methanol and NaCl solution, respec-
tively. The photopholatic parameters of the heterojunctions
were Fig. 13 and listed Table 2. The photovoltaic (PV) proper-
ties of the heterojunction at 10 mW/cm2 light intensity showed
that the short circuit current density Jsc for SnO2 NPs/Si
heterojunction prepared in NaCl solution was larger than that
of heterojunction prepared in methanol and the voltage open
circuit Voc was 0.5 V for both heterojunctions. The variation of
the photocurrebt with light intensity is shown in Fig. 14. The
photocurrent increasese as the light intensity increase and no
saturation in the photocurrent was observed indicates the fabri-
cated photodetectors have good linearity characteristics.

350
Methanol 1000
300
NaCl solution 250 100
200
Current (μA)

Current (µA)

150 10

100 Methanol
1
50 NaCl solution
0 0.1
-5 -4 -3 -2 -1-50 0 1 2 3 4 5
0.01
-100 Voltage (V) 0 1 2 3 4 5
-150 Voltage (V)
Fig. 11 Current-voltage characteristics of SnO2 NPs/p-Si heterojunctions Fig. 12 Semilogarithmic relationship of current-voltage characteristics of
prepared in methanol and NaCl solution SnO2 NPs/p-Si heterojunctions prepared in methanol and NaCl solution
Silicon (2021) 13:3229–3237 3235

Table 1 The electrical properties of the heterojunctions 0.6

Methanol
Heterojunction Io (μA) β Φ (eV)
0.5
NaCl solution
SnO2/Si (methanol) 5 3.8 0.68

Resposivity (A/W)
SnO2/Si (NaCl) 0.2 2.1 0.78 0.4

0.3

0.2

0.1

0
220 320 420 520 620 720 820
Wavelength (nm)
Fig. 15 Spectral responsivity plot of SnO2 NPs/p-Si heterojunctions
prepared in methanol and NaCl solution at 4 V

16
NaCl solution
Specific detectivity (Jones)×1010

14
Fig. 13 Illuminated I-V characteristics of n-SnO 2 NPs/p-Si Methanol solution
heterojunctions prepared in methanol and NaCl solution 12

10

6
Table 2 PV characteristics of heterojunctions
4
Photodetector Jsc (mA/cm2) Voc (mV)
2
SnO2 NPs/Si (methanol) 0.17 500 0
SnO2 NPs/Si (NaCl) 0.2 500 160 260 360 460 560 660 760 860
Wavelength (nm)
Fig. 16 Specific detectivity of SnO2 NPs/p-Si heterojunctions prepared in
methanol and NaCl solution at 4 V

3500

3000 NaCl solution

Methanol
Photocurrent (µA)

2500

2000

1500

1000 Table 3 Figures of merit of the photodetectors at 410 nm

500 Photodetector Rλ D* NEP EQE

(A/W) (Jones) × 1011 (pW)
0
0 10 20 30 40 SnO2 NPs/Si (methanol) 0.43 1.07 9.3 1.3
Light intensity (mW/cm2)
SnO2 NPs/Si (NaCl) 0.53 1.32 7.5 1.6
Fig. 14 Linearity characteristics of n-SnO2/p-Si photodetectors
3236
Figure 15 shows the spectral responsivity Rλ of the SnO2/
Si heterojunctions at reverse bias of 4 V. A sharp peak of
response was observed at 410 nm for the two heterojunctions
due to the absorption edge of the SnO2 film. The responsivity
of the photodetector prepared at NaCl solution was 0.53 A/W,
while it was 0.43 A/W at 410 nm for the heterojunction pre-
pared in methanol. The reason beyond this improvement can
be ascribed to large depletion layer width and due to large
surface area of the heterojunction prepared in NaCl solution
compared to that prepared in methanol. After 410 nm, the
responsivity decreases and then increases due to absorption
of the long wavelength in the silicon substrate. The diffusion
length and depletion region are extended into the silicon sub-
strate [32–34]. The external quantum efficiency EQE of the
photodetectors was calculated from responsivity data at 4 V
bias and found to be 1.6 and 1.3 at 410 nm for photodetectors
synthesised in NaCl and methanol, respectively.
The specific detectivity D* of the photodetector was deter-
mined from the following equation [35]
* Rλ ðAΔ f Þ0:5
D ¼ pffiffiffiffiffiffiffiffiffi ð4Þ
2qI o
Where A is the sensitive area of the photodetector and Δf is the
frequency bandwidth. Figure 16 shows the detectivity of the
photodetectors prepared in NaCl and methanol solutions.The
maximum value of detectivity of the photodetector was
1.32 × 1011 Jones for the photodetector prepared in NaCl so-
lution. The noise equivalent power NEP was calculated for
two photodetectors at 410 nm and listed in Table 3.
4 Conclusions
Tin oxide nanoparticles were successfully prepared by pulsed
Nd:YAG laser ablation in two types of solutions without using
catalyst. The effect of solution type on the size, size distribu-
tion and shape and optical absorption of SnO2 nanoparticles is
investigated. XRD studies show that the SnO2 NPs prepared
in NaCl solution have better crystallinity than that of synthe-
sized in methanol. The optical energy gap of SnO2 nanoparti-
cles prepared in methanol and NaCl were 3.95 and 3.8 eV,
respectively. SEM and TEM studies confirmed formation of
spherical nanoparticles and particles agglomeration was ob-
served. The electrical measurements revealed that the SnO2
NPs/Si heterojunction exhibited rectification properties and
the best junction characteristics were observed for
heterojunction prepared in NaCl solution. The maximum
responsivity was 0.53A/W at 410 nm for photodetector fabri-
cated in NaCl solution. The external quantum efficiency of the
photodetectors prepared in NaCl and methanol were 1.6 and
1.3 at 410 nm, respectively. The PV properties showed that
Silicon (2021) 13:3229–3237
the short circuit current density of SnO2 NPs/Si heterojunction
was larger than that of heterojunction prepared in methanol.
Acknowledgements The present study was supported via the Scientific
and Technological Research Council/ Turkey (TUBITAK)/ Department
of Science Fellowship/ Grant Programs (BIDEB)/ 2221– Fellowship
Program/ Visiting Scientists and Scientists on Sabbatical Leave (2019).
Also, it was supported by the University of Technology, Baghdad, Iraq.
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