Optical Fiber Technology 45 (2018) 122–127

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Optical Fiber Technology

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Soliton mode-locked thulium-doped fiber laser with cobalt oxide saturable T

absorber
⁎
H. Ahmada,b, , M.Z. Samiona, N. Yusoffa
a
Photonics Research Centre, University of Malaya, 50603 Kuala Lumpur, Malaysia
b
Visiting Professor at the Department of Physics, Faculty of Science and Technology, Airlangga University, Surabaya 60115, Indonesia

A R T I C LE I N FO A B S T R A C T

Keywords: In this work, we propose and demonstrate a mode-locked thulium doped fiber laser (TDFL) with an integrated
Mode-locking cobalt oxide (Co3O4) saturable absorber (SA). The SA is fabricated by suspending Co3O4 nanosheets in a polymer
Thulium film before being secured between two fiber ferules. The laser operates in the anomalous dispersion regime,
Cobalt oxide confirmed by the Kelly sidebands observed in the obtained optical spectrum. Mode-locking operation is obtained
Pulse fiber laser
at a low threshold pump power of 77.32 mW, with further optimizations made using a polarization controller
The laser generates pulses with a repetition rate of 11.36 MHz and a pulse width of 1.39 ps. The generated pulses
are highly stable, with a high signal-to-noise ratio of 46.00 dB and minimum power fluctuations indicating a
long-term stability. This work demonstrates a simple and a low-cost laser that would have potential applications
for operation near the 2.0-µm region, especially for medical applications.

1. Introduction metals [20,21], topological insulators (TIs) [22–24], transition metal

Passively pulsed fiber lasers are highly desired as laser sources due
to their potential use in a variety of applications ranging from material
processing to remote sensing, microscopy and medicine. The attrac-
tiveness of these sources arises from their robust yet compact form
factor, which in turn results low fabrication and operating costs [1–5].
To achieve this, fiber lasers are be designed to be either Q-switched or
mode-locked, with the latter generating shorter, ultrafast pulses with
overall low output energies and the former generating longer and
slower pulses but with higher energies [6].
Traditionally, Q-switching and mode-locking in fiber lasers was
achieved by actively modulating the losses within the laser cavity active
using acousto-optic or electro-optic modulators [7–11]. However, the
bulky nature of these modulators, as well as their relatively high cost
quickly made this option unsuitable for most real-world applications.
As such, research efforts were focused towards the development of
passively pulsed devices, which generated a similar output but in a
much more compact form factor and at a lower overall cost. This was
typically achieved primarily by saturable absorbers (SAs), such as
semiconductor saturable absorber mirrors (SESAMs) [12,13] and more
recently 2-dimensional (2D) and 3-dimensional (3D) materials such as
carbon nanotubes [14–16] and graphene [17–19]. Additionally, recent
developments have now seen new 2D and 3D nanomaterials, such as
dichalcogenides (TMDs) [25–27] and even exotic materials such as
black phosphorus [28–30] being used to obtain passive mode-locked
outputs. The fabrication and the nonlinear optical properties of these
low-dimensional materials have been widely investigated and reported
[31–33], with particular attention being paid to 2D nanomaterials for
advanced opto-electronic applications [34–36] due to their unique
properties such as low saturation intensity, broadband absorption
properties as well as fast recovery and response times [37–39].
Of late, transition metal oxides (TMOs) have now become the focus
of significant research interest for use as SAs due to their unique optical
charactersitics, namely their large nonlinear optical response [40]. As a
result of their 2D nature, the bandgaps of TMOs can be tuned without
altering their physical properties, giving them a wide-operational
bandwidth [41]. TMOs such as nickel oxide (NiO), zinc oxide (ZnO),
iron (II, III) oxide (Fe3O4), and titanium oxide (TiO2) have all been
successfully demonstrated as SAs for the generation of pulses fiber la-
sers [42–45]. The performance of these lasers is comparable to the ones
built using graphene or other 2D material based SAs, thus indicating the
potential of TMOs as SAs. In this regard, cobalt oxide (Co3O4) is an
attractive material for use as an SA as it has a large nonlinear to linear
absorption ratio [40], as well as spectral absorption that stretches to the
near-infrared (NIR) region [46]. Recently, the use of Co3O4 as an SA has
been reported with the generation of Q-switched pulses at the 1.5-µm

⁎
Corresponding author at: Photonics Research Centre, University of Malaya, 50603 Kuala Lumpur, Malaysia.
E-mail address: harith@um.edu.my (H. Ahmad).

https://doi.org/10.1016/j.yofte.2018.07.012
Received 6 April 2018; Received in revised form 22 May 2018; Accepted 2 July 2018
1068-5200/ © 2018 Elsevier Inc. All rights reserved.
H. Ahmad et al.
Fig. 1. (a) XRD pattern of Co3O4 nanosheets , (b) UV–vis spectra of the Co3O4-PEO in solution form with a close-up view of the absorption peaks (inset), and FESEM
images of the Co3O4 nanosheets taken at (c) low magnification and (d) at high magnification.
wavelength region [47]; however there are no reports yet on Co3O4
being used to generate mode-locked pulses in fiber lasers operating at
the longer 2.0-µm wavelength region.
In this report, a mode-locked thulium doped fiber laser (TDFL) using
a Co3O4 based SA is proposed and demonstrated for operation in the
2.0-µm region. Lasers operating in the 2.0-µm wavelength region are
‘eye-safe’, making them suitable for numerous industrial and medical
applications [48,49]. Furthermore, the strong absorption coefficient of
this wavelength region in water and gases makes them favorable for
various spectroscopy and sensing applications [50–52]. The TDFL is
configured with a thulium doped fiber (TDF) in a ring laser cavity as
well as an integrated SA. A polarization controller (PC) is also used to
optimize the laser's performance. The proposed setup has the advantage
of being easy to implement and does not require the use of costly and
difficult-to-handle modulators. This, combined with its operation in the
eye-safe region, gives the proposed system high potential for real-world
applications.
2. Fabrication and characterization of the SA
The Co3O4 nanosheets used in this work are obtained by the reac-
tions of a cobalt (II) acetate tetrahydrate [Co(CH3COO)2·4H2O] pre-
cursor, sodium hydroxide (NaOH), and polyethylene oxide (PEO). All
reagents are obtained from Sigma-Aldrich while an additional reagent,
ammonia (NH3·H2O) with a purity of 25%, is obtained from R&M
Chemicals. All chemicals are of analytical grade and used without any
further treatment.
The Co3O4 nanosheets used for the fabrication of the SA thin-film
are synthesized using the facile hydrothermal method. In this method,
the cobalt oxide precursor with a molar concentration of 2 mM is first
prepared by dissolving a sufficient amount of Co(CH3COO)2·4H2O in
deionized (DI) water by ultrasonication. Approximately 13 mL of NaOH
with a concentration of 3 mM is then added to the aqueous solution,
after which the solution is stirred continuously for another 30 min at
room temperature. The obtained solution is then mixed with 2 mL of
NH3·H2O using the drop-cast method and stirred at room temperature
for another 1 h. The suspended solution is then transferred into a
Teflon-lined stainless-steel autoclave and heated in a hot oven at 150 °C
for 16 h. After this, the mixture is left to cool at room temperature
123
Optical Fiber Technology 45 (2018) 122–127
before being centrifuged at 4000 rpm for 20 min to obtain the Co3O4
nanosheets structure, which appear as a black powder precipitate. The
Co3O4 nanosheet precipitate is then washed extensively with DI water
and absolute ethanol. This is repeated three times before the final
precipitate is dried in an oven at 60 °C for 24 h, giving the desired form
of a fine black powder.
While the nanosheets are the optically active material of the SA,
their fine and brittle nature does not allow them to be used in their
current form within the fiber cavity. As such, the Co3O4 nanosheets are
instead embedded in a Polyethylene-Oxide (PEO) thin film which serves
as a host material. The thin film is formed by dissolving 250 mg of PEO
powder in 30 mL of DI water, and stirred continuously at 50 °C for 2 h.
Approximately 10 mL of the Co3O4 black powder with a density of
5 mg mL−1 is then added into the PEO solution, and the entire mixture
stirred for another 2 h. The resulting compound is then transferred onto
a petri dish and left to dry in an oven at 60 °C for 24 h, forming a
polymer film with Co3O4 nanosheets embedded in the host material. A
small portion of the thin film formed is cut out and placed on the face of
a fiber ferrule so that it covers the core region. A small amount of index-
matching gel is used to hold the polymer piece in place, and another
fiber ferrule is then connected to the first using a standard fiber
adaptor. This forms the SA assembly which will be integrated into the
cavity of the proposed laser.
The synthesized Co3O4 nanosheets are characterized by x-ray dif-
fraction (XRD) using an Empyrean PANalytical x-ray diffractometer
with copper Kα radiation at an excitation wavelength of 1.5418 Å.
Diffraction peaks at 31.4°, 36.9°, 38.7°, 44.9°, 55.8°, 59.5°, and 65.4° are
obtained from the analysis, corresponding to the (2 2 0), (3 3 1), (2 2 2),
(4 0 0), (4 2 2), (5 1 1), and (4 4 0) planes of Co3O4 respectively as seen in
Fig. 1(a). All peaks are consistent with the JCPDS card 00-042-1467
[53], thereby confirming the successful synthesis of Co3O4. No other
significant peaks are detected in the spectrum, implying a high-level
purity in the fabricated compound. Furthermore, the narrow and high-
intensity diffraction peaks observed in the spectrum indicates a high
degree of crystallinity in the synthesized Co3O4 compund.
In addition to this, ultraviolet–visible (UV–Vis) spectroscopy ana-
lysis is also performed on the Co3O4-PEO when still in its solution form.
Characterization is carried out using a Varian Cary 50 UV–Vis
Spectrophotometer from Agilent Technologies over a wavelength range
H. Ahmad et al. Optical Fiber Technology 45 (2018) 122–127

of 200 nm to 800 nm. The resulting spectrum is given in Fig. 1(b), with
the linear absorption spectrum of the Co3O4-PEO solution exhibiting
four absorption peaks at the 233 nm, 286, 469 nm and 748 nm. The
peaks centered at 469 nm and 748 nm are attributed to the O11 → Co11
and O11 → Co111 bandgap energy transitions [54], and validate the
presence of the Co3O4 nanosheets in the PEO solution. The appearance
of another absorption edge at 286 nm is attributed to the semi-crys-
talline properties of PEO [55], and the combination of the individual
Co3O4 and PEO peaks shows the successful formation of the Co3O4-PEO
compound. The inset of the figure shows the same plot with a smaller
scale, with marker lines indicating the absorption peaks.
The morphological structure of the Co3O4 nanosheets are char-
acterized by Field Emission Scanning Electron Microscope (FESEM)
analysis. For this analysis, a Hitachi SU8220 FESEM operating at 2.0 kV
is used to capture the topographic details on the sample’s surface, with
the obtained images shown in Fig. 1(c). At low magnification, the
sample is observed to consist of many interconnected nanosheets with Fig. 3. The schematic diagram for the mode-locked laser operation in 2.0-µm.
irregular sizes, while at higher magnification it can be seen that the
sheet-like structures have an average diameter of less than 50 nm as and 6.2 µm at 2000 nm. Both ends of the TDF are connected to the
depicted in Fig. 1(d), confirming the nanoscale size of the fabricated common ports of the WDMs, with the LD connected to WDM1 config-
particles. Additionally, the image also shows that the fabricated sample ured for forward pumping, while the LD connected to WDM2 operates
consists of thick platelets with a high surface area. in the backward pumping configuration. A 2000 nm isolator is con-
For the non-linear absorption characterization of the fabricated SA, nected to the 2000 nm port of WDM2 to ensure unidirectional light
the twin detector technique is used to determine the SA’s modulation propagation in the cavity, and is in turn connected to 90:10 coupler
depth. For this analysis, a homemade mode-locked laser with a re- which is used to extract approximately 10% port of the propagating
petition rate of 28.169 MHz and a pulse duration of 2.33 ps is used as signal for further analysis. A polarization controller (PC), connected to
the seed laser for this measurement. A variable attenuator with a the output of the 90:10 coupler is used to optimize the signal propa-
maximum attenuation of 60 dB is used to vary the incident intensity on gating through the cavity. The PC is in turn connected to the SA as-
the SA for the characterization process. The modulation depth of the sembly, which is used to induce mode-locking in the propagating signal
Co3O4-PEO based SA is calculated to be around 43.7% as depicted in and is finally connected to the 2000 nm port of WDM1, thus completing
Fig. 2. This is comparable to the performance of other TMOs-based SAs the optical circuit.
[42,45], and thus shows that the fabricated SA in this work should be The laser cavity comprises of only single-mode (SMF-28) fibers and
able to generate the desired mode-locked output. The saturation in- the TDF that is used as the gain medium. Measurement of the fiber
tensity and the non-saturable loss of the SA is determined to be lengths gives a total cavity length of 18.3 m, consisting of the 4 m long
0.003 MW cm−2 and 56.3%, respectively. TDF and approximately 14.4 m of SMF-28 fibers. This consists of the
connecting fibers and also the various components used in the cavity. It
is important to note that the measured cavity length is only that of the
3. Experimental setup
ring cavity of the fiber laser, and does not include any components or
the SMF-28 fibers used to inject the pump signal into the ring cavity.
The schematic of the proposed mode-locked TDFL is given in Fig. 3.
The group velocity dispersion (GVD) of the TDF is −22.8 ps2 km−1 at
The TDFL is configured in a typical ring cavity with two Princeton
1958 nm as given by the manufacturer, while the GVD of the SMF-28
Lightwave 1560 nm laser diodes (LDs) used as the pump source. Both
fibers are calculated to be −68.4 ps2 km−1 at the same wavelength.
LDs have a maximum output power of 240 mW and each LD is linked to
Based on the GVD values of the TDF and SMF-28 fibers, the net cavity
a 1550 nm optical isolator before being connected to the ring cavity.
dispersion, D2 is computed as LTDFGVDTDF + LSMFGVD-
This is to protect the LDs from any damaging backscattering from the
SMF = − 1.0693 ps . As a result of this, the mode-locked laser is ex-
2
1550 nm port of the 1550 / 2000 nm wavelength division multiplexers
pected to operate in the anomalous dispersion regime.
(WDMs). The gain medium used is a 4-meter-long TmDF200 TDF, ob-
tained from OFS, with an absorption of 20 dB m−1 at 1550 nm and a
cutoff wavelength of 1350 nm. The TDF has a numerical aperture (NA)
4. Results and discussions
of 0.26, while the mode-field diameter of the fiber is 5.0 µm at 1570 nm

With fine adjustments made to the PC, mode-locked pulses are ob-
tained at a threshold pump power of 77.32 mW. Fig. 4(a) shows the
optical spectrum of the output laser obtained using a Yokogawa
AQ6375 optical spectrum analyzer at the threshold pump power. The
center wavelength of the laser is 1958.1 nm while its 3-dB bandwidth is
measured to be 3.25 nm. The presence of Kelly sidebands in the spec-
trum indicates that the mode-locked laser operates in the anomalous
dispersion regime. Based on the spectrum, the transform-limited width
of the generated pulse is calculated to be 1.24 ps using a time-band-
width product (TBP) value of 0.315 and assuming a hyperbolic-secant-
squared (sech2) pulse shape. In order to determine if the generated
mode-locked pulses are transform- or non-transform-limited, the posi-
tion of the Kelly sidebands with respect to the center wavelength (Δλ) is
determined both experimentally and theoretically. The value of Δλ
could be estimated from the equation [56,57]:
Fig. 2. Curve-fitted nonlinear absorption of the Co3O4-PEO SA.

124
H. Ahmad et al. Optical Fiber Technology 45 (2018) 122–127

Fig. 4. (a) Soliton mode-locked fiber laser spectrum, (b) theoretically calculated mth order of Kelly sideband positions in relation to the center wavelength (Δλ)
versus the pulse width (τp), (c) radio-frequency spectrum, and (d) pulse train of the mode-locked laser. All output characteristics of the fiber laser are taken at the
threshold pump power.

2
2 ln(1 + 2 ) λ2 4mπ ⎛ τp ⎞ −1
Δλ = ⎜ ⎟

2πcτp |D2 | ⎝ 2 ln(1 + 2)⎠ (1)

Fig. 5. The stability of soliton spectrum when tested over time.
Fig. 6. Autocorrelation trace generated by the mode-locked fiber laser and its
sech2 fitting curve.
where τp, λ, c, and D2 represent the pulse width, center wavelength,
speed of light and the net cavity dispersionrespectively. Fig. 4(b) shows
the plot of Δλ for the 1st, 2nd, and the 3rd order Kelly sidebands against
τp. For the transform-limited pulse width of 1.24 ps, the expected po-
sition of the 1st order Kelly’s sideband in relation to the center wave-
length is 6.3 nm, while its measured value is 6.1 nm. This slight de-
viation from the estimated value is attributed to pulse chirping [58],
however the magnitude of chirping cannot be determined in this work
due to the need to carry out sophisticated measurements which are
currently not available [59]. The radio-frequency (RF) spectrum of the
mode-locked pulse is obtained using an Anritsu MS2683A radio fre-
quency spectrum analyzer (RFSA) with a 12.5 GHz InGaAs photo-
detector at the highest resolution bandwidth of 300 Hz. The spectrum
obtained is given in Fig. 4(c) and shows a fundamental frequency peak
of 11.36 MHz. A high signal-to-noise ratio (SNR) of about 46 dB is
measured, indicating the generated output is highly stable [15]. The
pulse train generated by the mode-locked laser at a pump power of
77.32 mW is shown in Fig. 4(d), obtained using a Keysight DSOX3102T
1 Ghz oscilloscope. The average period of the pulses in the train is
measured to be 88.0 ns, corresponding to a repetition rate of
11.36 MHz. The pulse train has no significant fluctuations in the am-
plitude, maintaining an almost uniform shape and pulse intensity and
shows that the output pulses are highly stable. The repetition rate au-
gurs well with the estimated fundamental frequency for a cavity length
of 18.3 nm. Higher repetition rates can be obtained by using shorter
SMF-28 lengths to reduce the cavity round trip time.
To further determine the stability of the system, the output of the
mode-locked TDFL is obtained for a period of 60 min at constant room
temperature and without any external perturbations. The output is
measured at 5-minute intervals, with the composite spectra shown in
Fig. 5. No significant change can be seen in the spectrum obtained, with
a consistent spectral curve centered at 1958.1 nm observed over the
entire test period. The TDFL’s output shows only minor fluctuations in
its peak intensity, maintaining a value of around −25.7 dBm with a
fixed pump power of 77.32 mW. This shows that the mode-locked laser

125
H. Ahmad et al.
Table 1
Comparison of all-fiber mode-locked thulium doped lasers operating in the 2.0-µm wavelength region.
SA Threshold Pump Power Center Wavelength (nm)
(mW)
Black Phosphorus 300.00 1910.00
WSe2 650.00 1863.96
SWCNT 650.00 1947.00
Optically-deposited Graphene 130.00 1953.30
Graphene 400.00 1900.00
Co3O4 77.32 1958.10
is highly stable and is able to sustain long-term mode-locked operation.
Pulse width measurement is performed using a pulseCheck 150 USB
second harmonic generation (SHG)-based autocorrelator obtained from
A.P.E. at a fixed pump power of 77.32 mW. From the sech2 curve profile
given in Fig. 6, the pulse width is measured to be 1.39 ps, and when
combined with the spectral-bandwidth value of 3.25 nm, a TBP value of
0.353 is obtained. This is slightly higher than the transform limit of
0.315, again indicating that the pulse is chirped and also indicates that
the experimentally and theoretically measured Δλ value is not due to
negligible error. At the threshold pump power of 77.32 mW, the mode-
locked laser has an average output power of 0.11 mW, as well as a pulse
energy and a peak power of 9.43 pJ and 6.79 W respectively. At the
maximum pump power of 89.65 mW, a maximum average output
power of 0.26 mW is obtained, with a corresponding maximum pulse
energy and a peak power of 22.83 pJ and 16.43 W, respectively. Wang
et al. [57] had previously reported the use of a fiber amplifier with an
anomalous dispersion to amplify a 2 µm output pulse to induce an SHG
signal, but due to the fiber amplifier dispersion the amplified pulse
suffers from substantial pulse width broadening.
The measurement is conducted using a highly-sensitive detector
without the need of an amplifier, allowing the pulse width of the output
pulse to be measured without any significant broadening. The authors
are confident that this work can be further expanded towards achieving
shorter pulse widths using the CO3O4 based SA in a dispersion-managed
cavity with a net cavity dispersion close to zero or slightly normal to
generate pulses with shorter pulse widths [60]. Since most silica-based
fibers have anomalous dispersions at the 2.0-µm region, a normal-dis-
persion fiber (NDF) could be used in order to compensate the negative
dispersions of the other standard fibers, thus improving the generated
output. The center wavelength of the mode-locked laser can also be
tuned to be closer to the 2.0-µm region by either incorporating a tun-
able bandpass filter (TBPF), or a tunable Mach-Zehnder filter (TMZF).
Between these two, the latter provides an added advantage by main-
taining the soliton spectrum of the mode-locked laser in its original
form [61]. The use of a TBPF however would suppress the soliton mode-
locking due the limited bandwidth of the TBPF and hence cause the
pulse width to broaden [62].
The performance of the proposed Co3O4-based SA in this work is
comparable to that of other SAs used to generate mode-locked pulses in
similar fiber laser configurations. The comparison of the performance of
these SAs is given in Table 1.
It can be seen from Table 1 that the threshold pump power for this
work is significantly lower than that of most other works, which typi-
cally exceeds 300 mW. This is more than triple the threshold pump
power in this work, except for the case of the optically-deposited gra-
phene. This low threshold power is attributed to both the loss insertion
loss of the SA as well as the fiber cavity dispersion and the cavity length
[64]. The center wavelength of the mode-locked laser in this setup also
is the longest among those studied, at 1958.10 nm. The pulse width of
1.39 ps achieved in this work is comparable to those in other works,
ranging from 1.16 ps to 2.30 ps except when compared to black phos-
phorus which has a shorter pulse width of 0.74 ps. This however can be
addressed by managing the net cavity dispersion to be slightly normal.
The maximum pulse energy generated using the Co3O4 is also
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Optical Fiber Technology 45 (2018) 122–127
Repetition Rate (MHz) Pulse Width (ps) Maximum Pulse Energy (pJ) Reference
36.80 0.74 40.7 [28]
11.36 1.16 – [63]
16.00 2.30 18.8 [15]
16.94 2.10 80.0 [64]
19.70 1.90 69.30 [65]
11.36 1.39 22.83 [This work]
comparable to that obtained from the single wall carbon nanotube
(SWCNT) based SA, but falls short of others. In this regard, the proposed
laser setup can still be used as a seed laser source for optical amplifi-
cation to achieve the necessary output required for various industrial
applications [66].
5. Conclusions
In this work, a mode-locked TDFL with a Co3O4 based SA is de-
monstrated for operation in the 2.0-µm region. The Co3O4 based SA is
fabricated using Co3O4 nanosheets suspended in a polymer host and
sandwiched between two fiber ferrules. The mode-locked laser output
has a center wavelength at 1958.1 nm and a 3-dB bandwidth of
3.25 nm, as well as a repetition rate of 11.36 MHz, with a pulse width of
1.39 ps and SNR of 46.0 dB. The laser output is stable when tested over
a period of 60 min, with no observable shift in the center wavelength of
laser spectrum. The mode-locked laser would have multiple applica-
tions for operation at the ‘eye-safe’ region in 2.0-µm.
Acknowledgements
Funding for this research was provided by the Ministry of Higher
Education, Malaysia under the grant LRGS (2015)/NGOD/UM/KPT as
well as the University of Malaya under the grant RU 001–20017.
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