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Malaysian Journal of Science 43 (3): 13-21 (September 2024) https://mjs.um.edu.my

HYDROTHERMAL SYNTHESIS OF NITROGEN-DOPED CQDS OF RUBUS NIVEUS LEAVES FOR FLUORESCENT

pH SENSING AND PHOTOCATALYTIC APPLICATIONS
P. Negi1a, B.S. Rawat2b*, N. C. Joshi3c, W. Ahmad4d, N. Kumar5b, S. Upadhyay6e, K. P. S. Parmar7f, R. Saxena8g, R. Dhyani9h, P. S.
Khati10i, A.S. Rana11j

Abstract: The development of a fluorescent pH sensor and the treatment of wastewater with nanoparticles are both critical
topics. Variations in pH impact the morphology and subsequent properties of nanoparticles, affecting their utilization in
various fields, while using nanoparticles offers an improved approach for treating industrial waste. The present study
examines the effects of these variables on biologically produced nitrogen-doped carbon quantum dots (NCQDs). The
synthesis was achieved through a hydrothermal process using Rubus niveus leaf extract as a precursor. UV-Vis spectroscopy
analysis revealed absorption spectra over a wide range from 200 nm to 800 nm, with prominent peaks at 236 nm and 392
nm. Additionally, the direct energy band gap of the NCQDs was found to be 3.65 eV. SEM imaging displayed flower-shaped
particles, and FT-IR analysis indicated the presence of amide, CHO, N-H, and C-N functional groups. The XRD pattern revealed
that the surface morphology of NCQDs is amorphous in nature. A significant response in fluorescence intensity with varying
pH values was observed, confirming the potential of NCQDs as pH sensors. The reaction kinetics of Rhodamine-B (Rh-B) dye
was analyzed to assess the potential of NCQDs for dye degradation, revealing pseudo-first-order kinetics with a correlation
coefficient of 0.80.

Keywords: hydrothermal process, pH sensor, carbon quantum dots, energy band gap, dye degradation.

1. Introduction bioimaging, biomolecules (Ge et al., 2022; Basavaiah et al., 2018),

and metal ion sensors (Barati et al., 2016).
Carbon quantum dots (CQDs) are emerging as a promising The hydrothermal carbonization method is recognized as a
alternative to inorganic semiconductor materials due to their green synthetic approach for creating CQDs. Significant efforts
potential applications in various fields (Wang et al., 2016; Das et have been made to develop CQD fluorescent probes for metal ion
al., 2015; Bourlinos et al., 2013). Research highlights that low- detection and other applications (Du et al., 2013; Wang et al.,
toxicity, biocompatible, and chemically stable CQD materials are 2011; Lin et al., 2012; Liu et al., 2012; Salinas-Castillo et al., 2013;
useful in drug delivery (Jallel et al., 2018), optoelectronics (Hoan Mosconi et al., 2015; Pires et al., 2015).
et al., 2019), water treatment (Shamsipur et al., 2014), Doped CQDs offer tunable fluorescence and excellent surface
passivation. The incorporation of heteroatoms, such as nitrogen,
phosphorus, and sulphur, enhances the optical properties of
Authors information:
aDepartment of Chemistry, GRD Institute of Management & these particles (Carolan et al., 2017). Nitrogen-doped CQDs, in
Technology, Dehradun, UK, INDIA. particular, interact with carbon atoms by trapping radiating
bDepartment of Physics, School of Applied and Life Sciences electron-hole pairs, forming new optical centres, and exhibiting
(SALS), Uttaranchal University, Dehradun-248007, UK, INDIA. exceptional performance in optoelectronic, electro catalytic and
cDivision of Research and Innovation, Uttaranchal University,
luminescent applications. Carbon-bonded nitrogen introduces
Dehradun-248007, UK, INDIA. disorder into the hexagonal carbon rings (Li et al., 2012; Krysmann
dDepartment of Chemistry, Graphic Era University, Dehradun,
et al., 2012). The advantages of CQDs over organic fluorescent
UK, INDIA.
eDepartment of Allied Health Sciences, School of Health dyes include their biocompatibility, low synthesis cost, electron
Sciences and Technology, University of Petroleum and Energy transmission capability, water solubility, and ease of manufacture
Studies, UPES, Dehradun-248007, UK, INDIA. (Qu et al., 2010; Xiao et al., 2018; Zhang et al., 2016).
fDepartment of Physics, University of Petroleum and Energy
pH imbalances can cause various disorders by affecting the
Studies, UPES, Dehradun-248007, UK, INDIA. activity of several organelles, making precise measurement of
gDepartment of Physics, Shri Guru Ram Rai University,
intracellular pH crucial. Various materials, such as quantum dot-
Dehradun-248007, UK, INDIA.
hDepartment of Applied Science, Women Institute of encoded red fluorescent protein sensors (Tantama et al., 2011),
Technology, Dehradun, 248007, INDIA. Ag@SiO2 core-shell nanoparticles (Bai et al., 2013),
iDepartment of Chemistry, S.D.M. PG. College Doiwala,

Dehradun-248007, UK, INDIA.

jDepartment of Physics, Shri Guru Ram Rai (P.G.) College,
Received: July 25, 2023
Dehradun-248007, UK, INDIA. Accepted: September 19, 2023
*Corresponding Author: [email protected] Published: September 30, 2024

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semiconducting polymer dots (Chan et al., 2011), and fluorescent The current study focuses on the synthesis of nitrogen-doped
quantum FRET probe dots (Dennis et al., 2012), have been carbon quantum dots (NCQDs) from Rubus niveus leaves and
developed for pH monitoring. However, these materials have examines their characteristic properties, including their capacity
limitations including bulkiness, severe toxicity, and for photocatalytic degradation and fluorescent pH sensing.
biocompatibility issues. In contrast, CQDs have emerged as
excellent candidates for pH testing due to several advantages 2. Experimental Methods
(Han et al., 2010; Jin et al., 2010; Nie et al., 2014).
Moreover, prior studies have demonstrated that the presence Fresh Rubus niveus leaves were collected from a location near
of H⁺ or OH⁻ ions affects the morphology of biosynthesized metal the campus of Uttaranchal University. We employed
oxide nanoparticles (Zyoud et al., 2019). Changes in pH ethylenediamine and rhodamine-B without further purification.
significantly impact the hydrolysis and condensation processes Double-distilled to conduct the experiments
during the formation of the precursor solution (Arya et al., 2021).
These pH fluctuations similarly influence the morphology and 3. Synthesis of NCQDs
characteristics of biosynthesized nanoparticles, including their The synthesis of nitrogen-doped carbon quantum dots (NCQDs)
optical properties (Khairol et al., 2018). Recently, various plant was performed using a single-step hydrothermal method (Fig. 1).
parts have been shown to act as reducing and capping agents to Initially, the leaves were collected, washed with tap water,
create eco-friendly, non-toxic nanoparticles for diverse followed by deionized (DI) water to remove dust, and then dried
applications (Sathish kumar et al., 2012; Su et al., 2012; Su et al., in an incubator at ambient conditions. Subsequently, 5 g of the
2005). dried leaves were combined with approximately 60 ml of water
Rubus niveus, locally known as Kala Hisar or Mysore raspberries, and heated to 200 °C for 2 hours in a Teflon-lined autoclave. After
is a large, spiny shrub that commonly grows along highways, in this, 1.5 ml of ethylenediamine was added to 15 ml of the
woodlands, and in mountainous regions between 1000 and 2500 resulting carbon quantum dot (CQD) solution, which was then
m. It is noted for its antibacterial, anticancer, wound-healing, and subjected to further heating at 200 °C for an additional 3 hours.
anti-inflammatory properties. The phytochemicals responsible for Centrifugation was performed for about 45 minutes to remove
these unique qualities include saponins, tannins, flavonoids, large particles from the solution, followed by filtration using
phenols, and sugars (Blassan et al., 2014; Mullen et al., 2002). micro-level filter paper. The final solid product was obtained by
drying at 75 °C.

Figure1.Schematic of the synthesis of NCQDs

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4. Characterizations absorption bands were observed at 236 nm and 392 nm, with the
UV-Vis spectral analysis, Scanning Electron Microscopy (SEM), spectral range spanning from 200 nm to 800 nm. To estimate the
Fourier Transform Infrared Spectroscopy (FTIR), Energy Dispersive indirect optical energy band gap, the absorption spectrum was
X-ray Spectroscopy (EDX),and the X-ray powder diffraction (XRD) analyzed with reference to the absorption edge using the Tauc
method were employed to describe the powder morphology of equation (Tauc et al., 1966), a methodology well-documented in
NCQDs. the literature (Muhammad et al., 2011; Yakuphanoglu et al.,
2005). Theenergy band gap value estimation was performed by
Optical Properties Analysis plotting (𝛼ℎ𝜈)2 versus photon energy ℎ𝜈and found to be 3.65eV.
Analyses of absorption peaks, spectral ranges, and energy band
gaps were conducted at room temperature (Fig. 2). The

Figure 2.Plot of absorbance versus wavelength and (𝛼ℎ𝜈)2 versus hν

Figure 3. Plot of (a) absorbance and (b) emission versus wavelength in different solvents

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The photophysical properties of NCQDs were investigated and molecules' electronic transitions and energy levels. These findings
are illustrated in Figure 3. The plots of (a) absorbance versus suggest potential advantages for a broad range of industrial and
wavelength and (b) emission versus wavelength demonstrate the technological applications.
shift in peaks due to the use of different solvents, highlighting the
Solvatochromic effect of the synthesized particles (Khazan et al., SEM and EDX Analysis
2017; Dash et al., 1999). For solvents such as toluene, ethanol, The surface characteristics and morphological properties of
dioxane, and methanol, the peaks shift towards longer NCQDs were examined using scanning electron microscopy
wavelengths, indicating a bathochromic shift. Conversely, a (SEM). The SEM images of the NCQDs synthesized from Rubus
hypsochromic shift is observed with ethyl acetate and acetone, niveus revealed flower-shaped particles with some degree of
with N-hexane used as the reference solvent. agglomeration (Fig. 4a). The observed agglomeration may be
The solvent-dependent shifts are attributed to the solvents' attributed to the sample preparation process.
polarity and hydrogen bonding, which influence the fluorescent

Figure 4(a). SEM morphology of NCQDs

Figure 4 (b). EDX spectrum of NCQDs

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Figure.4 (b). Mapping of elements present in NCQDs

The EDX spectrum for analyzing the chemical composition of investigated using FTIR analysis. A prominent peak in the FTIR
NCQDs is presented inFigure4b. The graph displays the weight spectrum (Fig. 5) at 3390 cm-¹ corresponds to the N-H stretching
and atomic percentages of the four main elements: C, N, O, and vibration of secondary amines, indicating the presence of amino
K. The presence of both carbon and nitrogen indicates successful functional groups (Chang et al., 2022). The bands at 2932 cm-¹ are
incorporation of nitrogen into the CQDs. The detection of attributed to the Fermi resonance-induced C-H stretching of
potassium is attributed to an incomplete washing process, which aldehydes.
could be improved by washing with double distilled water and
ethanol before drying the material. The figure shows that carbon The C=O stretching of the amide group
constitutes the largest weight percentage. The presence of these resultsinabandat1650cm-¹, while the N-H bending vibration of the
elements without significant impurities confirms the purity of the amide is reflected in a troughat1548 cm-¹. The C-N stretching
synthesized NCQDs (Selva Raja et al., 2015). Elemental mapping vibration of the amine is responsible for the peaks at 1350 and
reveals a uniform distribution of these materials throughout the 1037 cm-¹, confirming the successful incorporation of nitrogen
synthesized NCQDs, as shown in Figure 4b. into the carbon dots. Furthermore, the FTIR data also verifies that
the CQDs are doped with nitrogen. The presence of these
Functional Groups Analysis functional groups, which also act as stabilizers, underscores their
The presence of functional groups on the surface of NCQDs, role in the formation of NCQDs, as observed in the plant extract.
which act as reducing agents during their synthesis, was

Figure 5. FT-IR spectrum for synthesized NCQDs

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Crystallographic Structure Analysis Analysis of p Effect on Fluorescence Emission

Figure (6) depicts the NCQDs' acquired XRD Figure 7a shows the produced samples, while Figure 7b
pattern. Comparison of the XRD pattern to the typical JCPDS card illustrates the measured fluorescence intensity of solutions at
no. 00-039-1405 reveals a large and powerful diffraction peak at various pH values. The significant shift in fluorescence intensity
2θ=21.367 with a hkl value of 220. with wavelength, observed as the pH value changes from 2 to 10,
This shows that synthesized NCQDs are amorphous. can be explained by the numerical excitation wavelength value of
the sample at 260 nm. The plot of fluorescence intensity versus
pH (Figure 7c), which yields a linear correlation coefficient of
0.771, further supports this association. This demonstrates that
the proposed NCQDs are promising candidates for pH
measurement applications.

Figure 6.XRD diffractogarm for synthesized NCQDs

Figure 7.(a)Prepared pH samples(b)Intensity of fluorescence versus wavelength (c)Intensity versus pH values

Photocatalytic Activity the dye concentration was monitored at 20-minute intervals

Their photocatalytic activity was evaluated under UV-visible using the peak of the pure dye as a benchmark. The results
light to assess the potential of the biosynthesized NCQDs for indicate that the dye concentration decreases gradually, though
degrading Rhodamine-B dye. During the experiment, a solution not significantly, over time (Figure 8b).
with a fixed concentration of the dye was used, and the procedure
was conducted without stirring the sample. The degradation of

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Figure 8. (a) Prepared samples of Rh-B dye (b)Plot of absorbance versus wavelength (c) Photocatalytic degradation efficiency of dye and (d)
Kinetic results for the degradation of dye

Figure(8c) illustrates the variation in photocatalytic degradation degradation was determinedtobe0.80, indicating its suitability for
efficiency over time. The kinetics of the degradation process was photocatalytic applications, with potential for further
analyzed to determine the photocatalytic decolourization's rate enhancement through additional treatment.
constant and correlation coefficient. The correlation coefficient
was found to be approximately 0.80, and the reaction rate 6. Funding
constant was determined to be 0.003min⁻¹ (Figure8d). The present work was carried out with the support of seed
money (Ref: UU/DRI/SM/2022/13) provided by Uttaranchal
5. Conclusion University, Dehradun.
Rubus niveus was utilized as the carbon source, and
ethylenediamine was employed to introduce nitrogen in the 7. Acknowledgement
hydrothermal method, successfully synthesizing NCQDs. Dr. B.S. Rawat, one of the contributors, expresses gratitude to
Characterization revealed the fluorescence properties, presence the Division of research & Innovation, Uttaranchal University,
of functional groups, and amorphous structure of the NCQDs. The Dehradun for facilitating the research facilities.
study demonstrated that this biocompatible material can produce
highly fluorescent particles. Additionally, the fluorescence
intensity varied with pH, confirming the potential of NCQDs as pH 8. Conflicts of Interest
sensors. The correlation coefficient for Rhodamine dye The author(s) declare(s) that there is no conflict of interest
regarding the publication of this paper

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