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ORIGINAL RESEARCH ARTICLE

A Study on Comprehensive Production Parameters

of Boron Nitride 2D Nanomaterial
Seval Hale Güler and Hasan Safa

Submitted: 27 February 2023 / Revised: 19 June 2023 / Accepted: 4 August 2023

In this study, BNNSs were synthesized via liquid-phase exfoliation method. Hexagonal boron nitride
powders were used as the starting material. The production of boron nitride nanosheets was optimized. For
this purpose, different sonication parameters and the effects of different solvents have been investigated.
Different sonication power and time parameters of the homogenizer (Sonics Vibra-cell VCX, 750 W) used
as the sonication parameter have been changed. In this stage, they were subjected to sonication process first
for 1-1.5-2 hours at 25% sonication power, 1-1.5-2-4 hours at 50% sonication power, and 1-1.5-2-4-6-8
hours at 75% sonication power. As a result of particle size analysis, time/sonication power parameters were
determined as 2 h-75%, 2 h-50%, 4 h-75%, 2 h-50%. The obtained samples were sedimented with cen-
trifuge process, washed with distilled water to remove solvent, and dried. Different solvents were compared
in the best power–time relationship. These solvents are dimethylformamide (DMF), isopropyl alcohol, N-
methyl pyrrolidone, ethylene glycol. The best results were obtained in DMF. The synthesized BNNS samples
were subjected to particle size (Malvern), scanning electron microscope (Zeiss, Gemini Supra 55), trans-
mission electron microscope (Jeol Jem-1011), Fourier transform infrared spectroscopy (Thermo Scientific
NicoletÔ iSÔ 5), Raman (WITech alpha 300R), x-ray photoelectron spectroscopy (Specs-Flex), and x-ray
diffraction analysis (PANalytical Empyrean).

The h-BN, which is the most common and stable allotrope,

Keywords artificial ceramic synthesis, boron nitride nanosheets
(2D nanomaterial), comprehensive synthesis
parameters, liquid-phase exfoliation method
1. Introduction
Boron nitride (BN), which is an artificial ceramic, contains
boron and nitrogen atoms. Boron and nitrogen atoms which are
adjacent to the carbon atom in periodic table are bonded with
carbon-carbon bonds as in graphite. Since boron and nitrogen
are adjacent to carbon, boron nitride is isoelectronic with
carbon and there is an isomorphism between them. Due to this
similarity, boron nitride has properties similar to carbon in
terms of many aspects along with polymorphs and crystallo-
graphic phase transformations (Ref 1). Boron nitride is a
material having superior properties in terms of chemical,
electrical, and thermal properties. In general, it is obtained as a
result of reaction of boric acid or boron oxide with carbon and
nitrogen gas or organic carbon and nitrogen carriers (Ref 2).
The polymorphs of BN are as follows: hexagonal BN (h-BN)
having sp2 bond, rhombohedral BN, cubic BN (c-BN), and
wurtzite BN (w-BN) having sp3 bond. In addition, 1D boron
nitride nanotube (BNNT) and 2D hexagonal boron nitride can
be considered as polymorphs in nanosheets and these can be
synthesized from h-BN (Ref 3).
Seval Hale Güler, Rare Earth Element Application and Research
Center, Munzur University, Tunceli, Turkey; and Hasan Safa,
Metallurgical and Material Engineering Department, Mersin
University, Mersin, Turkey. Contact e-mail: sevalhale@gmail.com.
is the form in which B-N atoms form strong bonds and are
arranged in layers and these layers overlap to form a three-
dimensional arrangement. Since layers are bonded to each other
with weak bonds in three-dimensional arrangement, these
materials show lubricant and soft properties. Because of this
property, it is widely used as a lubricant and filler material in
cosmetic products (Ref 4). Hexagonal boron nitride (h-BN) has
many interesting features such as low-density structure, elec-
trical insulation, high thermal stability and conductivity, perfect
inertness, and low friction coefficient. h-BN has a wide
bandwidth; therefore, it usually has a white appearance and it
tends to be transparent when the layer thickness is reduced.
Since the hexagonal boron nitride nanostructures are located in
the visible region of 390-700 nm in electromagnetic spectrum,
they do not exhibit any optical absorption. Besides, the
ultraviolet (UV) range shows a peak in the range of  210-
220 nm (Ref 5). The electronic band structure of the hexagonal
boron nitride is still discussed. In the literature, bandwidth
value was found to vary between 3.6 and 7.1 eV (Ref 6). It is
possible to increase thermal conductivity of the composite by
adding iron oxide nanoparticles into the h-BN layers. One of
the biggest and most successful applications of h-BNs is its use
as a filler to thermally conductive polymers. BN layers are
estimated to have a higher thermal conductivity (k) than their
counterparts. Out-of-plane vibrations contribute to the reduc-
tion of phonon scattering in 2D layers. This explains the
difference in heat transfer constant between a single-layer and
bulk h-BN (Ref 7).
In addition to graphene, another potential two-dimensional
nanomaterial is the boron nitride nanosheet (BNNS). Like
graphene oxide (GO), BNNSs show superior thermal and
mechanical properties. BNNSs are separated from h-BN into

Journal of Materials Engineering and Performance

layers by using chemical or physical methods (Ref 8). In the
last decade, when multilayer BN nanosheet and single-layer BN
nanosheet (BNNS) are compared with graphene, they attract a
great attention due to its wider energy band gap, unique
physical, chemical, and electrical insulation properties (Ref 9).
In addition, boron nitride nanosheet (BNNS) has been proven
to show better performance than its bulk counterparts in the
fields of solid lubrication, transistor, and composite-filling
materials (Ref 10). BNNS can be produced by micromechanical
cleavage of BN crystal (Ref 11), opening of BN nanotubes (Ref
12), chemical vapor deposition (CVD) (Ref 13), and exfoliated
bulk BN powder (Ref 14). The widely applied chemical
processes cause a considerable number of surface defects that
generally reduce mechanical and chemical stability of BNNSs.
In physical exfoliation, exfoliation, ball milling, or ultrasoni-
cation is used in order to separate BNNSs into layers from h-
BN (Ref 8). Boron nitride has an ideal surface energy of about
65 mJ/m2, and thus, BNNS is generally produced in solvents
such as isopropyl alcohol (IPA) or N-methyl pyrrolidone
(NMP). This holds true for most of 2D materials with an energy
of about 70 mJ/m2 (Ref 15). When compared with mechanical
exfoliation and CVD method, liquid-phase exfoliation is low
cost and provides high efficiency. In fact, liquid-phase exfo-
liation is a general definition because different methods are
used for different approaches. Liquid-phase exfoliation method
contains ion penetration, ion exchange, and sonication-sup-
ported exfoliation method. Liquid-phase exfoliation method is
an easier method unlike other methods. Nanosheets can be
obtained by putting the material into some solvents and using
appropriate ultrasonic parameters. Besides, there are many
solvents that can be used; therefore, it is very important to
choose the appropriate solvent. According to the standard
solution theory, stability of the solution can be determined by
the ionization and polarizability of different components (Ref
16). These methods used in the production of BNNSs such as
mechanical cleavage, chemical method, and liquid-phase
sonication were preferred at the end of the process since the
crystallinity of pure h-BN is conserved greatly and the layers
are easily separated. Numerous studies have been conducted to
determine its stability in solutions as well as production
methods in order to obtain single-layer BNNS with high
amount and high quality for application purposes (Ref 17). In
order to figure out the distribution ability of 2D materials,
Coleman et al. (Ref 18) and Bergin et al. (Ref 19) worked on
these materials by using Hansen solubility parameter theory.
They claimed the necessity of reduction of enthalpy distribution
for a good solvent or solvent mixture. Therefore, exfoliation
energy is minimized (Ref 15). Zhou et al. (Ref 20) showed that
they could achieve a highly stable and layered BNNS
suspension using a mixture of solvent such as water and
ethanol (Ref 21). In their studies, Wu et al. (Ref 22) and Zhi
et al. (Ref 23) found that dimethylformamide (DMF) (surface
energy 37.1 mJ/m2) exhibited polar-polar interaction with the
h-BN surface in order to separate effectively BN particles into
layers. This interaction breaks the Van der Waals bonds
between the h-BN layers.
As a result, BNNSs can be well dispersed in many solvents
such as chloroform 0.3 mg/mL and DMF 0.7 mg/mL in
solvents (Ref 4). Pacile et al. (Ref 24) first studied on the
synthesis of BN nanostructures, and Han et al. (Ref 25) studied
on the production of double- and single-layer BN sheets.
However, the production efficiencies in these studies were
limited due to the restrictions on production methods used (Ref
23). In conclusion, LPE method is a promising method for the
mass production of BNNSs. In previous studies in the literature,
many different results have been obtained. The main reason for
this situation is that the parameters used in those studies differ
significantly. Therefore, the production conditions were opti-
mized first in this study and BNNS synthesis was made with the
solvents by which the best results were obtained in the literature
by using these optimized conditions. Thus, the solvents used
for production of BNNS were compared with each other.
2. Materials and Method
In the study, Merck brand hexagonal boron nitride powder
(1 lm, 98%) was used as the starting material for the
production of boron nitride nanosheets. In this study, ethyl
alcohol (Merck, 99.8%), N,N-dimethylformamide (Sigma-
Aldrich, 99.8%), ethylene glycol (Merck, 99.8%), N-methyl-
2-pyrrolidone (Sigma-Aldrich, 99.8%), and 2-propanol (Merck,
99.8%) were used. BNNSs were synthesized by using liquid-
phase exfoliation method. For BNNS production, as seen in
Fig. 1, 0.07 gram h-BN powder and 100 ml DMF were
subjected to sonication process according to the parameters
determined in a beaker. When the solvent atoms were
penetrated into the layers of h-BN material during sonication
process, the weak Van der Waals bonds between them were
broken. In BNNS production from h-BN using liquid-phase
exfoliation method, h-BN was subjected to sonication process
in the determined time and power in an ultrasonic homogenizer
in the solvent. In the first stage of this study, BNNS was
produced at the times and sonication powers determined in
Table 1 in order to determine the optimum production
conditions by using DMF. In this stage, they were subjected
to sonication process first for 1-1.5-2 hours at 25% sonication
power, 1-1.5-2-4 hours at 50% sonication power, and 1-1.5-2-4-
6-8 hours at 75% sonication power. The obtained samples were
sedimented with centrifuge process, washed with distilled water
to remove DMF, and dried. Particle size analysis was conducted
to the samples and kept on waiting for sedimentation analysis.
In accordance with the results, it was found that sufficient
efficiency was not obtained at 25% and 50% sonication power
with sedimentation and particle size analysis. It was observed
that the sample sonicated for 2 h at 75% sonication power was
produced in nm dimensions with the desired efficiency.
Therefore, the optimum parameters were chosen as 75% power
and 2 hours. In the next process, the production was made over
the solvent and parameters specified in Table 2. BN powders
were mixed with the time and power determined with the help
of ultrasonic homogenizer (Sonics Vibra-cell VCX 750 W) in
the solvent in Table 2. The obtained samples were subjected to
centrifuge process for 120 minutes at 5000 rpm. It was then
washed 4 times with distilled water. The obtained powder
mixture was dried at 150 °C in an oven. The synthesized
BNNS samples were subjected to Particle Size (Malvern),
scanning electron microscope (SEM) (Zeiss, Gemini Supra 55),
transmission electron microscope (TEM, Jeol Jem-1011),
Fourier transform infrared spectroscopy (FTIR, Thermo Scien-
tific NicoletÔ iSÔ 5), Raman (WITech alpha 300R), x-ray
photoelectron spectroscopy (XPS, Specs-Flex), and x-ray
diffraction analysis (XRD, PANalytical Empyrean).
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Fig. 1 The production stages followed in this experimental study

Table 1 Experimental production parameters in different time/sonication power

Materials Sonication time, h Sonication power, % Centrifuge Time/h

1 25
1 50
1 75
1.5 25
1.5 50
Dimethylformamide(DMF) 1.5 75 2
2 25
2 50
2 75
4 50
4 75
6 75
8 75

Table 2 Experimental production parameters in different solvents

Materials Sonication time, h Sonication power, % Centrifuge time, h

Dimethylformamide (DMF) 2 75 2
_
Isopropyl alcohol (IPA) 2 75 2
Ethylene glycol (EG) 2 75 2
N-methyl pyrrolidone (NMP) 2 75 2

3. Results and Discussion
One of the important observations made in nanomaterials is
sedimentation. The sedimentation rate of a nanomaterial
distributed homogeneously in a liquid can give information
about the particle size of the material. In this study, the obtained
samples were first examined by conducting sedimentation
observation. Since the density and surface tension of different
solvents are different, they will exhibit different sedimentation
times even for materials with the same properties. Firstly, the
produced boron nitride nanosheets were dispersed in ethanol
order to eliminate these differences and standardize the
observation.
One of the analyses conducted in BNNS production stages
with liquid-phase exfoliation method is the sedimentation
observation. In this analysis, the size comparison can be made
by calculating the sedimentation time of the produced samples
in the solvent depending on time. In the first stage, the samples
given in Table 1 were subjected to sedimentation analysis as
seen in Fig. 2 and the sample produced by using 75% power
was determined to be the sample that had the longest
sedimentation time as seen in Fig. 2 This is an indication that
there are high amount of nm-size BN layers with low thickness
in the structure. Sufficient nanosizes could not be achieved in
the samples produced by using 25 and 50% sonication power in
BNNS production compared to graphene. However, the desired
dimensions were obtained at 75% sonication power. Figure 2
shows the time-dependent sedimentation image of the product
obtained at different times such as 4, 6, and 8 hours at 50-75%
constant sonication power. The sedimentation time decreased
with increasing sonication time. This can be attributed to the
increasing size of BNNS layers reduced to nanosizes by their
agglomeration with increasing time. As a result of particle size
analysis (Fig. 3), time/sonication power parameters were

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Fig. 2 Sedimentation analysis
determined as 2 h-75%. Weak Van der Waals interactions
between BN layers are stronger than graphene, and thus, liquid-
phase exfoliation process of h-BN is more difficult. In the
literature, it is stated that the amount of nanosheet to be
produced with increasing sonication power increases (Ref 26,
27). This leads to interactions named ‘‘lips–lips’’ between
adjacent BN layers.
Zhi et al. (Ref 23) reported that BN particles should be
dissolved in DMF in order to obtain pure BNNS structures
having average nano-sheet thickness after centrifugation.
Successful completion of the liquid-phase exfoliation process
can be associated with the strong interaction between DMF and
BN surfaces. Besides, Coleman et al. (Ref 18) proposed a series
of different solvents such as NMP and IPA based on Hansen
solubility theory in order to exfoliate h-BN (Ref 28).
The morphologies of pure BN powder and stratified BN
were investigated using SEM and TEM analysis. When Fig. 4
is examined, it is clearly seen that hexagonal boron nitride
was successfully separated from each other in general without
any broken layer and these layers have a single-layer array
along with their transparent structure. In addition, the layers
that were in agglomerated form in the starting powder were
successfully dispersed and the goals like deagglomeration,
dispersion, and grain refinement were successfully achieved
(Ref 29).
SEM image shows nanosheet-like structures and the pres-
ence of particles with much smaller sizes that stuck on these
layered structures (e-g). In addition, the images show that
geometric forms were the nanosheet-like structures. It is clearly
understood from the images that these sheet structures were
separated into their layers. As a result of the dimensional
measurements taken on the images, it was determined that the
obtained particles were in the form of flat sheets (platelet) and
their dimensions were approximately 30, 50, and 70 nm. In
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Fig. 3 Particle size analysis
Fig. 4(b), it was seen that there was no residual nanoparticle on
the boron nitride nanosheets and their surfaces were quite clean.
This confirmed that the optimum time-power correlation for the
produced BNNSs was 2 h and 75% power. It reached up to 30,
50, and 70 nm in some places and up to several hundred nm in
some other places. The layers around 30 nm are thought to be
formed by breaking the large layers. The layers seen to be in
different widths were determined to be in different sizes from a
few lm to a few hundred lm. It was determined that BN was
separated into layers and their width and height ratio was high
and there was no distortion in the lateral areas. It was also seen
that BNNSs can be obtained from BN powder by interactions
between BN particle surfaces and solvent molecules with
sonication process. When the non-exfoliated particles were
compared, not only the particle thickness but also the lateral
sizes of BN layers decreased. This result indicated that a BN
nanosheet can be successfully synthesized by sonication
process (Ref 30).
Figure 4 shows TEM images too. It can be easily seen that
the contrast in the regions shown in the images is quite
transparent compared to the bundle-BN islets that had a size of
about 500 nm and can be seen with a darker (black) contrast in
the image. The obtained TEM analysis results were confirmed
by the TEM images obtained from different studies (Ref 29).
Here, the structures similar to the regions determined with TEM
contrast in the images are quite similar to the BNNS images
recorded in previous TEM studies. Therefore, from this point of
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view, it can be said that liquid-phase exfoliation technique
successfully separated layers of h-BN and provided the
formation of BNNS. Much more interesting thing is that more
fringes were visible in the regions marked in TEM images
recorded in both low magnifications as stated in Fig. 4(b). This
obtained structure is a structure having grid-like gaps. This
proves that the layers overlap. While a transparent image was
obtained in some regions, contrast darkness increased in some
regions. More fringes, which were much more visible in the
images, actually provide evidence for the formation of BNNS
islets becoming bundle by overlapping the regions seen in
black contrast. Another interesting point in the images is that a
BNNS(s), having a transparent contrast that can be expressed as
a ghost, was noticeable though just barely (Ref 29).
At this point, it can be clearly seen based on the nano-sized
and detailed TEM results that liquid-phase technique can be
used in the production of BNNS from h-BN. As seen in figures,
nanoparticles composed of nanolayers having approximately
the same size morphologically (Ref 31).
Fourier transform infrared (FTIR) spectroscopy is an
analysis type used to determine different functional groups on
chemical structures (Ref 32). Figure 5(a) and (b) shows FTIR
analysis of BN nanosheets synthesized by liquid-phase exfo-
liation. BNNS peaks obtained as a result of the production of h-
BN by using liquid-phase exfoliation method were seen to be at
1335 and 760 cm 1. The peak at about 1335 cm 1 was caused
by sp2 bonds, and the peak at around 760 cm 1 was caused by
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b Fig. 4 Production of BNNS (a) in DMF solvent at
sonication power SEM and TEM, (b) in DMF solvent at
sonication power SEM and TEM, (c) in DMF solvent at
sonication power SEM and TEM, (d) in DMF solvent at
sonication power SEM and TEM, (e) in IPA solvent at
sonication power SEM and TEM, (f) in NMP solvent at
sonication power SEM and TEM, (g) in EG solvent at
sonication power SEM and TEM
Fig. 4 continued
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2 h-50% the vibrations in B-N-B bonds. In their study, Hao et al. (Ref
2 h-75% 33) stated that h-BN intra-plane B-N bond formed an
4 h-50% absorption band at 1435 cm 1 in FTIR spectra of boron nitride
4 h-75% nano-bars. In their study on boron nitride nanotube synthesis,
2 h-75%
Dai et al. (Ref 34) found h-BN peaks at 1377 and 819 cm 1 in
2 h-75%
2 h-75%
the FTIR spectrum of the samples in their study on synthesis of
boron nitride nanotube. In addition, the peak at 1377 cm 1 was
attributed to the sp2 bond of B-Ns and the peak at 819 cm 1
was attributed to the bond forming h-BN structure with out-of-
Fig. 5 FTIR spectrum (a) different sonication power, (b) different solvent
Fig. 6 XRD results of h-BN and BNNS
plane B-N-B bond. The results obtained from the present study
are compatible with the results obtained in the previous studies,
and it was observed that there were BNNS structures having h-
BN crystal lattice in the structure. The fact that the results are
close to the literature information indicates that the structure is
h-BN (Ref 31). In Fig. 5(a), the difference between 1330 and
1345 cm 1 in the FTIR analysis for different sonication powers
is seen. Figure 5(b) shows FTIR results of the samples obtained
by using different sonication parameters in different DMF
environment, and the peaks were very similar to one another
since there were in the same solvent medium. In Fig. 5(b), the
solvents are compared and FTIR analysis results of the
sonication process made with 75% power for 2 hours are
given. In line with the obtained results, it was observed that the
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Table 3 FWHM values of XRD results
XRD samples FWHM data, °
2 h-50% 0.26
2 h-75% 0.27
4 h-50% 0.28
4 h-75% 0.29
_
Isopropyl alcohol 0.29
Ethylene glycol 0.29
N-methyl pyrrolidone 0.29
Untreatment h-BN 0.02
isopropyl alcohol, N-methyl pyrrolidone, and ethylene glycol
solvent gave a characteristic peak in the range of 1320 and
1347 cm 1 unlike DMF. The reason of these peaks is thought
to be the solvent residues in the material during the rinsing
process of the solvents used (Ref 35-37).
Figure 6 shows XRD pattern of exfoliated BNNS powders
obtained by using x-ray diffraction. When the images were
examined, characteristic 4 peaks were found in all samples in
general. When XRD for BNNS sample was examined, previous
studies were seen to be very close to each other compared to the
experimental result. XRD characteristic bands were observed at
expected intervals (Ref 38, 39).
It was seen that XRD results had crystal reflections (002),
(100), (102), and (004). When the Bragg angles of these peaks
were examined, BN peak was seen at 2h value as 26.8° (Ref
39). Compared to the untreated BN powders, exfoliated h-BN
exhibited four similar characteristic peaks with decreased
density. These peaks were 26.7°, 42.1°, 50.5°, and 55.4° peaks
at (002), (100), (102), and (004) planes. The (002), (100),
(102), and (004) peaks of BNNSs show a significantly reduced
intensity. The weakened diffraction peaks indicated that the
layered BNNSs crystallized at low small dimensions and
showed a noticeable decrease in the structure array and the thin
BN layers were stacked weaker in the sample (Ref 4).
When h-BN and BNNS XRD spectra were compared, it is
clear that the peaks did not change in both materials in terms of
diffraction angle and shape, which shows that high-pressure
homogenization and exfoliation process did not damage the
crystal structure of the pure material. It conserved the high-
crystalline structure of the BN mass (Ref 40).
When the width of h-BN peak given in Fig. 6 and FWHM
value (Table 3) were examined, it was determined that while the
peak width was low, the peak width of the BNNS samples
produced with liquid-phase exfoliation method was high and
the FWHM values were high.
The crystallographic properties of the BNNS synthesized by
the liquid-phase exfoliation method were determined by the
XRD (x-ray diffraction) technique, and the obtained XRD
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spectrum is as given in Fig. 6. As known from the literature, the
peak width is associated with the size of the crystal. XRD
analysis of BNNSs revealed that BNNSs were in  99% purity
and in crystalline phase (Ref 31). In their study, Li et al. (Ref
41) found diffraction peaks of (002), (100), (110) planes at 25°,
43°, and 78° and Zheng et al. (Ref 42) captured the peaks of
(002), (100), (110) planes in XRD analysis of synthesized
boron nitride structure in another study; thus, they stated that
the structure was hexagonal boron nitride. In their study on the
effect of temperature on the characteristic of boron nitride
structure, Shi et al. (Ref 43) stated that the peaks of (002),
(100), (101), (004), (103), (104), (110), (112), and (006) planes
were involved in JCPDS (Joint Committee of Powder Diffrac-
tion) card no. 34-0421 in the standards.
Raman spectroscopy has appeared as one of the character-
ization tools for many materials and gives information about
the Raman spectrum and structural and phase information (Ref
44).
The Raman results obtained from the produced samples
given in Fig. 7 are approximately 1366 cm 1. Raman active
E2g mode was caused by B and N atoms moving against each
other in the plane and planar atomic displacements (Ref 7).
There is a typical Raman spectrum in the range of 1200-
1500 cm 1 for h-BN with single crystal; the Raman peak is
associated with E2g phonon mode and occurs at a maximum
width of 1366 cm 1 and the height of 8.1 cm 1. In particular,
sp2 is caused by the planar vibration of the hybridized B-N-B
bond. This peak is intense and narrow in BNNS and shows
defective structures with low concentration (Ref 40, 45, 46).
This reveals that the high-pressure homogenization process is
effective in making finer particles such as BNNS from bulk
material (Ref 37). The reason for the Raman peak to be at
1366 cm 1 in h-BN structure is the elongation of bulk h-BN
and B-N bonds because of the interaction between the layers
after exfoliation process (Ref 47). FWHMs of E2g peak points
of untreated h-BN were compared with FWHMs of layered
BNNS used during the experiment, and it was found that there
were wider FWHMs ( 18.5 cm 1) for BNNSs layered by
using DMF solvent. Similarly, FWHM of the widest layered
BNNSs obtained from the solvents used belonged to DMF.
When the layers in the intact h-BN were compared with those
of BNNSs, the thinnest layers were seen to be obtained.
FWHM of the solvents used such as IPA, NMP, and ethylene
glycol used was found to be  15.8 cm 1 (Ref 17). The D-
band peak of boron nitride can be defined using a Lorentzian
peak. As can be understood from the data, the Raman spectrum
of the produced boron nitride powder showed its highest peak
at 1366 cm 1. This spectrum is compatible with studies in the
literature (Ref 5).
XPS survey (Fig. 8a) shows the coexistence of B and N as
main elements and O as impurities in the samples (Ref 48).
Figure 8(a) shows that the sample surface consists of N, B, and
O with binding energies of N1s, B1s, and O1s at 392.3, 191.4,
Fig. 7 Raman results of h-BN and BNNS
and 532.5 eV, respectively. Figure 8(a) shows typical B1s, N1s.
The B1s spectra in Fig. 8(b) are identified to be B-N peak at
191.4 eV and B-O peak at approximately 192.2 eV which
originates from the hydroxidation of some boron atoms at the
surface of the sample. The results obtained are compatible with
the literature (Ref 49).
One of the characterization methods used to identify the
presence of defects in boron nitride nanosheets and the
chemical bond composition of BNNSs is the x-ray photoelec-
tron spectroscopy. According to XPS results, B and N were
main elements and O and C were present as the impurities in
the samples. B/N ratio was found to be close to the values
obtained in the literature (Ref 48) and it was found to be
approximately 1.07. The peak at  391 eV in the N1 spectrum
was attributed to the N-B bond (Fig. 8c). Approximate values
were obtained for all samples.
4. Conclusion
SEM analysis was performed in order to display the
hexagonal boron nitride layers separated from each other in
the nano-layered boron nitride structure obtained with liquid-
phase exfoliation process. When the images were examined, it
was clearly seen that the liquid-phase exfoliation process
successfully separated the hexagonal boron nitride layers and
these layers were in a single-layer array with transparent
structures obtained from TEM results. It was found to be
composed of nanosheet-like structures synthesized with SEM
and TEM analyses supporting each other.
In exfoliation process, sonication and solvent effect are two
determining factors. Raman microscopy also confirmed the
presence of a few-layer sheets by determining the peak shift
compared to pure h-BN, and these results are supported with
TEM images. The crystallinity of the obtained h-BNNS was
determined with XRD analysis, and the peak of h-BN was
clearly seen which was confirmed by the result that the effect of
ultrasonic power in h-BN synthesis gave a better result. In
FTIR analysis, it was determined which element and which
bond structures are present in the synthesized nanoparticles and
it was concluded that hexagonal boron nitride nanosheet
production with high purity was achieved as a result of all
characterization studies. It was confirmed that the peak at
around 1335 cm 1 was caused by B-N bonds and the peak at
around 760 cm 1 was caused by the vibration in B-N-B bonds.
These results were supported by the XPS results obtained. It
was seen that the layers were bundled with the increase of
sonication time for the same sonication power. In the sonication
used in low power, it was observed that the layers were not
completely separated and the agglomerated h-BN structure did
not deteriorate.
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Fig. 8 XPS spectra of the BNNS samples. (a) Survey spectrum; (b) B1s; (c) N1s

Journal of Materials Engineering and Performance

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