Applied Surface Science Advances 11 (2022) 100308

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Applied Surface Science Advances

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A novel temperature dependent method for borophene synthesis

Mohammad Asaduzzaman Chowdhury a, *, M.M. Kamal Uddin a, Md. Bengir Ahmed Shuvho b,
Masud Rana a, Nayem Hossain a, c
a
Department of Mechanical Engineering, Dhaka University of Engineering & Technology, DUET, Gazipur 1707, Bangladesh
b
Department of Industrial and Production Engineering, National Institute of Textile Engineering and Research (NITER), Savar, Dhaka 1350, Bangladesh
c
Department of Mechanical Engineering, International University of Business Agriculture and Technology (IUBAT), Dhaka 1230, Bangladesh

A R T I C L E I N F O A B S T R A C T

Keywords: In energy, sensor, and biomedical applications, borophene is considered as an emerging and promising material.
Boron However, since bulk boron exhibits rather intricate spatial structures and multiple chemical properties, the
Borophene synthesis of borophene is yet to be considered as a challenging issue. A large amount of theoretical work has been
Novel method
conducted to characterize the properties of borophene incorporating the possible experimental methods. Un­
Electrochemical exfoliation process
fortunately, synthesis of borophene and their properties in experimentation do not comply the theoretical ex­
Cathode design
pectations within the desired level. There are some methods that have been used to synthesize borophene but
these techniques also have some limitations such as complexity and expensive. Due to this reason, the seeking of
new methods continues even now a day. In this research, a novel method has been proposed. This method is
nearly similar to the electrochemical exfoliation process of graphene production. Nevertheless, graphite is
conductive at ambient temperature, whereas boron is almost insulating at low temperature. Therefore, a new
design is explored with the boron attached heating coil so that it can act as a conductive material with increasing
temperature and confirmed the synthesis of borophene from boron by electrochemical exfoliation process. The
quality and crystallographic structure of anisotropic borophene with the change of temperature will also be
followed by this method. Apart from the pure boron rod, the sintering process is utilized under different aspects
to develop the boron structure under optimum conditions. The crystallographic structure of boron can be
changed by the sintering process under different operating and processing parameters. The synthesis of bor­
ophene from various crystallographic structures of boron will provide the new insight of borophene for its use in
large scales. This new method of borophene synthesis is practically conducted at a limited level, still needs more
analysis by using advanced characterization techniques. The Raman spectrum of fabricated borophene is eval­
uated and stability of this borophene is tested by using zeta potential. This method can be considered as a most
promising and potential method in comparison with the other available techniques.

1. Introduction technological platform embedded with artificial intelligence for intelli­

2D materials (2DMs) have attracted a paramount interest for better
anode materials in metal-ion batteries. 2DMs exhibit distinctive optical
and electronic properties and outstanding applications in electronics,
optoelectronics, energy storage and conversation and sensing have been
studied since the discovery of graphene in 2004 [1]. Sensors’ sensing
capacity is enhanced due to the tremendous electronic properties,
incomparable surface area, and tunable surface chemistry. Recent
research has shown that neither pure metal carbides/nitrides (MXenes)
nor polymers (P) are able to resolve the practical problems of sensors [2,
3]. In particular, 2D materials-based biosensors are now becoming a new
gent systems such as medical diagnostics [4,5]. Nevertheless, 2DMs
properties and structures have been designed and studied, novel
methods are still ascertained in applied research, in particular bor­
ophene for sensor applications. In the future, borophene may be used,
like MXenes, as electrochemical biosensors for health issues, especially
cancer detection because of its high surface area, presence of surface
functional groups, and electrical characteristics [6]. Moreover, bor­
ophene has good prospects in biomedical applications even though they
are still challenging [7].
Borophene, which is considered to be the general class of 2D boron
sheets, obtains in various phases such as rhombohedral and rectangular

* Corresponding author.
E-mail addresses: asadzmn2014@yahoo.com, asad@duet.ac.bd (M.A. Chowdhury).

https://doi.org/10.1016/j.apsadv.2022.100308
Received 15 July 2022; Received in revised form 5 September 2022; Accepted 20 September 2022
Available online 23 September 2022
2666-5239/© 2022 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
M.A. Chowdhury et al. Applied Surface Science Advances 11 (2022) 100308

phases [8]. It has significant mechanical and anisotropic electronic Table 1

properties, tunable gap, superconductivity, notable energy storage ca­ Comparison between existing and new borophene synthesis processes [13,14,7,
pacity, and good chemical stability. Moreover, this 2D material is 15–20].
exclusive from carbon materials which usually have a layered structure Process Temperature range Nature of Borophene producedas
[9]. Complexity appears during synthesis of borophene because of boron
complex structure and electron inferiority of boron. Borophene is a 2D Chemical
structured boron sheet identical to graphene with distinctive physico­ vapor deposition
chemical properties. Some abrasives, such as carborundum, are hard Molecular- 300 to 1100OC In As a coating layers on
beam epitaxy powder different substrates, it is
enough to scratch (9.3 on the Mohs scale), but too brittle to be used in
form difficult to use where
tools. It makes up roughly 0.001% of the Earth’s crust by weight. Boron only borophene is
is found in a variety of forms, including borax, kernite, and tincalconite important, stability level
(hydrated sodium borates), which are the most common commercial is different for different
boron minerals found in California’s arid regions, as well as widely substrate materials.
Ion Structural configuration:
dispersed minerals like colemanite, ulexite, and tourmaline. Sassolite, or implantation
natural boric acid, is found primarily in Italy. There are at least four (plasma
crystalline variations or allotropes of pure boron. The various crystalline based)
forms of elemental boron feature closed cages containing 12 boron Cu γ − β28
foil
atoms grouped in an icosahedron. Very few experimental studies on
Ag β12 and X3
borophene preparation have been explored because of complex elec­ (111)
tronic structure and electron inferiority of boron which could lead to Al honeycomb
many complexities during borophene synthesis. Chaudhary et al. [10] (111)
found that the study on borophene synthesis utilizing direct exfoliation Si β
(001)
is least investigated because of network bonding complexity of boron.
N/A β−
The higher shielding efficiency of nanosheets compared to other rhombohedral
samples is greatly connected to their high conducting values, which are Liquid phase N/A Suspended in liquid
primarily influenced by the amount of silver nitrate utilized during exfoliation solution
(unstable, difficult to
production [11]. This discovery provides a new door for commercial
characterize, not usable
core-shell topologies that incorporate borophene to protect electro­ practically)
magnetic pollution. The nucleation obstacle is the main barrier since it Present method Temperature between Circular Solid particle
controls the formation of borophene and it depends on the specific 600 to 1000◦ C rod (stable like graphene
growth temperature which is considered a key parameter to the syn­ exfoliated boron and particle, commercially
borophene flakes are viable and used in the
thesis of borophene [12]. When the synthesis temperature is signifi­
seen. Moreover, the applications where pure
cantly low, boron growth is unable to defeat the nucleation obstacle of temperature more borophene is important).
the 2D structure. On the other hand, high temperature can govern the than 1000◦ C will also Borophene structure has
synthesis of borophene by conquering the nucleation barrier of boron. be observed, since the been traced by Raman
melting temperature Spectroscopy Test
Thus, growth temperature requires a novel control method which could
of boron is 2,200◦ C.
lead to locating the free energy of boron growth between the nucleation
obstacle of the 3D boron and 2D borophene. The aim of this research
work is to explore the simple borophene synthesis process. In this acids, platinum is inert; however, in aqua regia, it dissolves. Hydrogen
research work, borophene is collected and analyzed. The existing and embrittlement isn’t a concern. It’s one of the few rare metals that can
new borophene synthesis processes are shown in Table 1 in comparison withstand seawater chlorides properly. Ionic liquids, aqueous acids, and
with the present method. aqueous inorganic salts can be used to electrochemically exfoliated
boron similar to graphite as electrolytes.
2. Materials and method

2.1. Materials 2.2. Existing methods and challenges

Boron is the only semiconductor element in Group IIIA, the fifth
element in the periodic table, with valence orbitals comparable to car­
bon and adjacent to it. Because of these similarities, borophene, a lit 2D
metal, could have interesting properties similar to graphene. Because of
its unique electrical structure, complicated bonding mechanisms, and
strong resemblance to carbon components, borophene is expected to
have great qualities similar to graphene and even it can perform better
as a new super material. Pure crystalline boron is a black, glossy semi­
conductor, which conducts electricity like a metal at high temperatures
but acts as a near-insulator at low temperatures. The properties of boron
are atomic number: 5, atomic weight: [10.806, 10.821], melting point:
2,200◦ C, boiling point: 2,550◦ C, specific gravity: 2.34 (at 20◦ C),
oxidation state: +3 and electron configuration: 1s22s22p1. In the elec­
trochemical exfoliation method, boron is designed to utilize as a cathode
material. Platinum is a favored anode material due to its low con­
sumption rate and strong electrical conductivity. Platinum is preferred
for an anode’s outer surface because it is corrosion resistant and can
maintain current flow in most electrolyte solutions without forming an
insulating layer, resulting in a lower consumption rate. In fused salts and
Beyond graphene, synthetic organic chemists are still trying to figure
out a way of making scalable synthesis of elemental two-dimensional
(2D) materials [21]. The manufacturing of borophene is troublesome
since 3D boron bonding configurations are accompanied by a high en­
ergy difference as compared to the 2D form. In addition, borophene
synthesis usually requires extremely low pressures and advanced
equipment. Even back then, borophene synthesis was achievable using
the bottom-up approach, top-down approach, exfoliation techniques (i.
e., sonochemical, liquid phase, and micromechanical exfoliation),
deposition techniques such as chemical vapor deposition (CVD) and
physical vapor deposition (PVD), ion-intercalation, solvothermal/hy­
drothermal methods and so on [13,14,7]. It resulted in a variety of
borophene complexes that were either supported by a substrate or
freestanding. Due to the bonding topologies in bulk boron, synthesizing
borophene is still a major issue. A triangular lattice with periodic holes
and the ability to grow on metal substrates, in particular Ag (111), Au
(111), and Cu (11) should theoretically be more stable. Borophene has
previously been produced on single crystals of silver or copper, but these
substrates are tiny, costly, and unsuitable for studying transport

2
M.A. Chowdhury et al.
properties or electronics applications [15]. The overview of the existing
methods is illustrated in Fig. 1. The temperature range for producing
borophene is within the range of 300 to 1100◦ C with different structural
configurations, properties and applications [13,14,7,15–20].
As previously stated, the molecular beam epitaxy (MBE) method is
better for fabricating monolayer or few-layer high-crystallinity bor­
ophene, whereas the CVD method is better for controlling the layer or
structure configuration of large-area borophene with various standing
directions to the substrate. The sonication-assisted liquid-phase exfoli­
ation process, which has a more hopeful future in industry, is recom­
mended for high-yield borophene. Only a few borophene phases have
been successfully manufactured up to this point, significantly less than
the many dozen predicted in theory. As a result, the researchers continue
to face a significant challenge. The wavy shape of borophene due to its
unique atom packing, is making it labor intensive for researchers to
produce stable borophene using mechanical exfoliation methods. As a
result, preparation tactics for borophene synthesis are shifting to alter­
native techniques such as solvothermal method, liquid-phase exfolia­
tion, BME, CVD, PVD. However, synthesis of borophene is still
challenging, because bulk boron has fairly complex spatial arrange­
ments and various chemical characteristics [16]. The sonochemical
exfoliation process [9,17–20] is a distinct technique and fully different
from the proposed novel process. In sonochemical synthesis,
free-standing borophene sheets were made by dispersing 150 mg of
boron in 40 ml each of the following: acetone, di-isonopropyl alcohol,
di-methyl formamide, iso-propyl alcohol, and ethylene glycol. Every
bottle was placed in an ultrasonic bath (Cole Parmer, 40 KHz), and the
dispersion was ultrasonically treated for up to 24 h. In order to guar­
antee the production of borophene sheets, samples were obtained
regularly, from every two hours to twenty-four hours, from each of the
five vessels containing various solvents. Following centrifugation (Remi,
R-24) of the resultant fluids at a speed of 5000 rpm for three minutes,
optical and transmission electron microscopy were used to analyze the
supernatant. The technique was continued in order to produce few layer
borophene sheets as it was discovered that the supernatant includes
fewer than 8 layers. The difficulty of filtering out borophene from the
reaction solution in sonochemical synthesis can be overcome with the
help of the suggested technique.
Fig. 1. An overview of existing method for synthesis of borophene.
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Applied Surface Science Advances 11 (2022) 100308
2.3. Proposed novel method
This novel method for borophene is based on the concept of graphene
synthesis from the electrochemical exfoliation process which is illus­
trated in Fig. 2 which is completely different from the concept of
sonochemical exfoliation process [9,17–20]. Comparing with graphene
synthesis, graphite is used as a cathode material. In reality, graphite is a
carbon-based filler with an electrical conductivity of 104 S/cm at
ambient temperature, which is comparable to carbon fibers. Due to its
good electrical conductivity, it can produce a large amount of exfoliated
graphene at low temperature, which makes the process less chemical
tedious, faster, easier, and scalable. However, in borophene synthesis
boron can be used as a cathode material in this proposed electro­
chemical exploration process. The problem is that boron is not a good
conductor like a graphite at low temperature. Boron is nearly an insu­
lator at low temperature; however, it conducts electricity similar to a
metal at high temperature [22–24]. The electrical conductivity of boron
at ambient temperature is only 0.0001 S/m. To resolve this constraint,
boron is designed in such a way so that the temperature of boron can be
varied.
In this design, a hollow opening in the circular boron rod was
maintained and the electric heater coil was inserted in this opening. The
temperature controller was connected with this boron rod to control the
temperature of boron at a desired level. In the electrochemical exfolia­
tion process, the platinum as an anode and designated boron as a
cathode were immersed in a suitable electrolyte solution. The temper­
ature of the boron rod was increased at a certain level and conductivity
was measured to maintain the conductivity within the required level
which exfoliates borophene.
Afterwards, through the vacuum filtration, the exfoliated borophene
flakes were congregated from the electrolyte solution. It was filtered
several times by porous nylon membrane and washed with demineral­
ized water for removing any trace of residual salts from the collected
boron flakes.
Exfoliated boron flakes were sonicated for a minimum two hours in
acetone so that flakes could disperse into it and produce a few atomic
layers of borophene. Subsequently, the sonicated solution was centri­
fuged for 30 min at 4000 rpm to separate the atomic layers of borophene
and boron flakes. As a result of that centrifugal force, boron flakes are
M.A. Chowdhury et al. Applied Surface Science Advances 11 (2022) 100308

Fig. 2. Novel method of borophene production (all machines, such as temperature controller, heating coil, centrifuge and sonication are available in our laboratory).

deposited as a dross in the test tube where the supernatant part of the process is conducted without any vacuum conditions. In the future, the
solution contains only a few atomic layers of borophene. Finally, the synthesis of borophene by this novel process will be conducted under
supernatant solution of layered borophene was collected by decantation. vacuum conditions to avoid the adverse effects of environmental
The wet borophene was then dried and collected for further investiga­ contaminants.
tion. The advantage of this novel process is that the borophene can be
produced at various temperatures. The optimum temperature condition
for confirming better quality of borophene can be identified. This
method also exhibited the advantages of less chemical tiresome, faster,
easier and scalable similar to graphene manufacturing. The synthesis

Fig. 3. Borophene particle after sonication.

4
M.A. Chowdhury et al.
3. Results and discussion
3.1. Physical observation and Raman spectroscopy analysis
This method is practically conducted recently in our laboratory,
temperature between 600 and 1000◦ C exfoliated boron and borophene
flakes were noticed. After sonication, borophene particles are visible
shown in Fig. 3 in acetone solution and this solution was collected in a
centrifuge tube for centrifugation as seen in Fig. 4. The Raman spectrum
of borophene obtained in this method is confirmed by literature [25]
and almost similar trend is observed as represented in Fig. 5. This test
can be considered as a trial-and-error basis and more tests and analysis
are required for clear understanding of the prospect of this method for
in-line mass production, stable borophone and commercial aspects. The
behavior of electrolyte solution with the increase of temperature in
terms of viscosity and conductivity is not examined during this initial
test.
3.2. Stability analysis
Any particle in suspension, macromolecule, or material surface ex­
hibits the physical characteristic known as zeta potential. To evaluate
the potential stability of the colloidal system, zeta potential is used. In
zeta potential, the first inner layer of the electric double layer, which
occurs at a charged surface in an ionic solution, is known as the Stern
layer. The Stern layer, which is made up of a layer of ions charged in
opposition to the surface and adhering to it, is stationary with respect to
Fig. 4. Solution of borophene for centrifugation.
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Applied Surface Science Advances 11 (2022) 100308
the surface. The next is diffuse layer by which both positive and negative
ions are existed loosely. Considering all layers, the stability of any par­
ticles is measure within the slipping plane. The stability level can be
positive or negative depending on the particle tested. The block diagram
of surface charge zeta-potential is illustrated in Fig. 6.
For borophene sample, the zeta potential value is above +100mV,
represents sample excellent stability. Where the borophene particle size
was found 400 to 600 nm. The standard table of zeta potential for
confirming the stability is noted in Table 2.
4. Prospects and possible challenges
The challenges of this novel method are:
(i) Temperature management is necessary for situating the free en­
ergy of boron growth between the nucleation obstacle of 3D
boron and 2D borophene. So far, there are no graphs or tables to
find the relationship between temperature and electrical con­
ductivity of bulk boron. The temperature seems to be conductive
after 600◦ C (from a recent test) although the conductivity is not
measured. However, there is a relationship graph of electrical
conductivity and resistivity against temperature for boron-
undoped (NCM-1) and boron-doped (NCM-2) nanoceramic pel­
lets depicted in Fig. 7 [26]. This Figure may provide some insight
of the temperature behavior on boron but this may not be the
naked truth.
(ii) Despite the electrochemical exfoliation process, boron was
designed with the electrical coil for varying the temperature.
How the electrolyte solution will behave with increasing tem­
perature is not examined in this preliminary analysis. Neverthe­
less, it can be noted from previous results and confirmed that the
amount of an electrolyte dissolved in solution is influenced by
temperature. Higher temperatures improve electrolyte solubility
and thus, ion concentration, resulting in greater electrolytic
conduction [27]. Fig. 8 illustrated the trends of the results where
electrolyte solution is a function of molar concentration and
temperature. The quality of the electrolyte solution and their
viscosities change cannot be assured before application of this
new method.
(iii) The quality, structure and properties of produced borophene by
this method is expected to be better but these can be assured after
TEM, FESEM, EDS, Zeta Potential, XPS, XRD, FTIR, AFM, UV,
Particle size analysis and other related observations.
(iv) According to earlier research [25], borophene can be anisotropic,
and as a result, their electrical conductivity varies depending on
the crystallographic orientation. This is another challenging issue
and also it can be considered as a hopeful consequence since it
exhibits higher carrier density and mechanical stiffness in
preferred direction because of this property.
5. Conclusions
The novel method of borophene production can be used as an
alternative technique among the processes available in literature. This
process followed in this method is less expensive and simple, although
the temperature control is the challenging issue since the increase of
temperature of boron converts it from insulator to conductor. The other
technologies can be adopted with this system by which the insulator is
transformed into a conductor despite the fact that these processes are
not applied for boron [28–30]. Recently (July, 2022), some preliminary
synthesis process was conducted as a trial basis and some hopeful in­
sights were found. The borophene was confirmed by Raman spectros­
copy. The stability was measured by Zeta potential and excellent
stability was obtained. For newly proposed 2D materials, stability is an
important aspect for experimental realization and large-scale produc­
tion. Temperature is also an important thermodynamic variable for
M.A. Chowdhury et al. Applied Surface Science Advances 11 (2022) 100308

Fig. 5. Raman spectrum of borophene (a) present study (b) literature [25].

Fig. 6. Block diagram of surface charge zeta-potential.

determining the stability of materials. At higher temperatures, the

Table 2
phonon modes are occupied according to Bose–Einstein statistics. The
Zeta potential for stability range.
change of crystallographic structure of boron rod with increasing tem­
Zeta potential Magnitude (mV) Behavior of Stability perature and the sintering process of manufacturing boron rod in porous
0 to − 5
+ Rapid coagulation or flocculation or nonporous structure may also have some role to change the stability
− 10
+
to +
− 30 Incipient instability of borophene in a desired level as compared to existing borophene
− 30
+
to +
− 40 Moderate stability produced by the methods available.
− 40
+
to +
− 60 Good stability
However, the process is continuing and repeating several times for
>+ − 60 Excellent stability
the confirmation of the method’s success. The article is proposed only
for this method and in-depth characterization of produced borophene
will be expected to be considered in the next article.

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M.A. Chowdhury et al. Applied Surface Science Advances 11 (2022) 100308

Fig. 7. Electrical conductivity and resistivity against temperature for boron-undoped (NCM-1) and boron-doped (NCM-2) nanoceramic pellets [26].

Fig. 8. Electrolyte solution as a function of molar concentration and temperature [27].

Declaration of Competing Interest
[7]
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
[8]
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