SYNTHESIS AND CHARACTERIZATION of CARBON QUANTUM

DOTS (CQDs) FROM RAMBUTAN LEAVES EXTRACTS FOR

Cu2+ DETECTION

Andini Fikarda1, Laksmi Dewi1*, Isnaeni2*, Nonni Soraya Sambudi3*

1
Chemical Engineering, Universitas Pertamina, Jakarta Selatan, Indonesia

*
Corresponding author: Laksmi Dewi S.T, MS., Dr.Isnaeni, Dr Nonni Soraya Sambudi

1*
Chemical Engineering, Universitas Pertamina, Jakarta Selatan, Indonesia

2*
Reseach Center for Physics, Group of Applied Laser and Theoretical Physics, LIPI,
Tanggerang, Indonesia

3*
Chemical Engineering, Universiti Teknologi of Petronas, Perak, Malaysia

E-mail address: laksmi.dewi@outlook.com1*, isnaeniusman@gmail.com2*,

nonnisoraya@gmail.com3*
Synthesis And Characterization Of Carbon Quantum Dots (CQDs)
From Rambutan Leaves Extracts For Cu2+ Detection

A facile, rapid, eco-friendly, and frugal approach was developed for the
preparation of highly fluorescent Carbon Quantum Dot (CQDs) by hydrothermal
and microwave treatment of Rambutan Leaves as a carbon source. The effects of
leaves condition and various synthesis methods on the physical and optical
properties of CQDs, and also the sensing activity of CQDs through copper ion
addition were studied. The properties of as-synthesized CQDs were analyzed by
using UV- Vis Spectrophotometer, Photoluminescence Spectroscopy, and
Fourier-Transform Infrared spectroscopy (FT-IR). The results showed that CQDs
preparation from Rambutan leaves via hydrothermal and microwave treatment
have been successfully synthesized by exhibiting light brown solutions. In this
study, the band-gap energies of CQDs were found to be 3.51 eV - 2.52 eV
indicating that CQDs had semiconductor characteristic. The CQDs solutions
portrayed significant fluorescence property in which bright blue-green (cyan)
fluorescence can be observed by naked eye under Ultraviolet (UV) light
irradiation (405 nm). The dried Rambutan leaves-hydrothermal-based CQDs
offer the highest quantum yield of 2.70%. The FT-IR analysis showed the
formation of CQDs that predominantly consists of carbonyl and hydroxyl groups
on a surface, which can provide more adsorption sites for Cu 2+ adsorption
process. Furthermore, this study indicated that the sensitivity of CQDs emission
from dry Rambutan leaves - hydrothermal showed the best turn off behavior
when detecting the presence of copper metal ions with a minimum LOD as low
as 123 µM. Thus, the presented sensing system is reliable to be used as sensing
method and for other analytical applications.

Keywords: Rambutan leaves; hydrothermal synthesis; microwave synthesis;

Carbon Quantum dots (CQDs); green synthesis; Cu2+ ion detection; fluorescence
sensor
Introduction

Integration of principles of 'Green Chemistry' in nanoscience such as Carbon

Quantum Dots (CQDs) has attracted researchers in recent years. Carbon dots (CDs),

also called Carbon Quantum Dots (CQDs), are a new type of zero-dimensional (0D)

photoluminescent nanocarbon with a size range less than 10 nm [1]. The synthesis of the

CQD process is simple, and the raw materials are low-cost. Due to their low toxicity,

high chemical stability, good biocompatibility, and good light stability, CQDs have

potential applications in many fields such as biomarkers, bioimaging, biosensing, drug

[2]
delivery, ion detection, optoelectronics and photocatalysis . Besides, the CQDs

preparation method has abundant carbon source and simple reaction equipment.

The synthetic methods for CQDs are generally classified into two main groups:

top down method and bottom up method. Top down method used graphite material as

nanocarbon source, while Bottom up used organic molecules to synthesis CQDs, such

as acid, carbohydrate, biomaterial, polymer, silica, dan composite [3]. Some of top down

method to synthesize CQDs: for example, laser ablation, arc discharge, electrochemistry

oxidation, combustion, and pyrolysis. Meanwhile, microwave and hydrothermal process

are classified as bottom up method [4].

But most of the methods are complicated, costly, and toxic. The toxic substances

used in the experiment have always been the problem that researchers are eager to

solve. For example, laser ablation and arc discharge are complex and costly, while

chemical oxidation is toxic due to strong acid using in CQDs synthesis process. As a

result, the hydrothermal and microwave process for CQD synthesis can be the best

choice due to its simplicity, low cost, controlled reaction conditions, fast methods, and

environmental friendly [5].

 Clean and green synthesis based method was chosen as the CQDs preparation

method for this study. CQDs synthesis used carbon sources from natural and renewable

material. There are many advantages of using natural material as carbon sources such as

non-toxicity, clean, and abundant source. Some literature which has used natural
[6] [7] [8]
materials for CQDS synthesis, such as soybean , pamelo peel , orange juice ,

green-grass [9], potato [10], plant leaves [11], soy milk [12], and silk cocoon [13].

In this study, CQDs will be synthesis through the hydrothermal and microwave

method from Rambutan leaves with variations of CQDs material condition. Rambutan

leaves were chosen due to its abundant sources and high contents of glucose, fructose,

and sucrose [14].

Experimental Section

Apparatus and Reagents.

Rambutan leaves was washed with pure water and aquabidest then a half of Rambutan

leaves was dried in oven at 90 °C for 6 hours. Rambutan leaves was grinded into

powder.

Hydrothermal autoclave Teflon and microwave were used to synthesize CQDs form

Rambutan leaves. A fluorescence spectrophotometer and a UV-VIS spectrophotometer

were used to record fluorescence spectra and absorption spectra of CQDs, respectively.

A Fourier Transform Infra-Red Spectroscopy (FT-IR) was used to observe the

functional groups on a surface CQDs.

Synthesis of Rambutan leaves CQDs through hydrothermal method.

The preparation process of CQDs is shown in Figure 1-A&B. Firstly, 150 mg of dried

and fresh Rambutan leaves powder was taken and dissolved into a 50 mL of double-

distilled water (Aquabidest) in a beaker and transferred into a 50 mL of Teflon-lined

autoclaved and kept it for 5 hours at 200 °C. The obtained solution was cooled down to

room temperature (RT) naturally. The black-brown carbonaceous material was

centrifuged up to 8,000 rpm for 15 minutes to remove the larger particles. CQDs

synthesis were done in duplo.

Synthesis of Rambutan leaves CQDs through microwave method.

The preparation process of CQDs is shown in Figure 1-C&D. Firstly, 300 mg of

blended fresh and dried Rambutan leaves were taken and dissolved into a 100 mL of

double-distilled water (Aquabidest) in a beaker and transferred into a microwave and

kept it for 30 minutes at 360 watt. The obtained solution was cooled down to room

temperature naturally. The black-brown carbonaceous material was centrifuged up to

8,000 rpm for 15 minutes to remove the larger particles. CQDs synthesis were done in

duplo.
 Figure 1. Process routing of CQDs

Characterization of CQDs.

The luminescence and absorption properties of samples were determined by a

fluorescence spectrophotometer and an ultraviolet spectrophotometer. The functional

group on the surface of the samples were observed and determined using a FTIR.

Detection of metal ion by CQDs.

The fluorescence spectra of CQDs were recorded in the presence and absences of Cu 2+

metal ions with various concetration (50 µM, 100 µM, 200 µM, and 400 µM) at the

excited wavelength of 405 nm.

Result and discussion

The experiments were done with two variations of CQDs material condition which are

dried and fresh Rambutan leaves through two different synthesis method which are

hydrothermal and microwave. Each of experiment was done in duplo.

Hydrothermal method synthesis.

Figure 2-A&B shown physical characteristic result of CQDs after hydrothermal process

from dried and fresh Rambutan leaves. These two as-synthesized CQDs showed
different liquid color before and after hydrothermal treatment. The DRL-CQDs (Dried

Rambutan Leaves-CQDs) showed to be light brown liquid while the DRL-CQDs (Fresh

Rambutan Leaves-CQDs) obtained to be dark brown liquid. The obtained color change

indicated that the carbonization process has been successfully carried out, which is

identified from previous solution to be more concentrated solution, as has been done by

previous literature[15]. The possible mechanisms for converting Rambutan leaves into

CQDs through hydrothermal method can involve several processes, such as hydrolysis,

dehydration, condensation, aromatization, and carbonization[8].

Figure 2-C&D shown visual test using the UV laser from the excitation wavelength of

405 nm. The emission wavelength from both DRL-CQDs and FRL-CQDs tended to

emitted visible cyan to light blue. However, DRL-CQD possess brighter emission

compared to others. Both sample have similar results with previous literature where

emission wavelength from spinach-CQDs[16] and Tamarindus Indica-CQDs[17] tended to

release bright blue and cyan emission.

Figure 2. The physic characteristic of CQDs through hydrothermal method from (A)
DRL-CQDs and (B) FRL-CQDs ; The emission of CQDs through hydrothermal method
from (C) DRL-CQDs and (B) FRL-CQDs
Microwave method synthesis.

Another method was done for CQDs synthesis method. Figure 3-A&B shown physical

characteristic result of CQDs after microwave process from dried and fresh Rambutan

leaves. The DRL-CQDs and FRL-CQDs exhibited different liquid color before and after

microwave treatment. The DRL-CQDs possess yellow brown liquid while the DRL-

CQDs exposed darker yellow brown liquid. The obtained color change indicated that

the carbonization has been occur perfectly during microwave treatment, which is

identified from previous solution to be more concentrated solution, although the liquid

were less concentrated than CQDs from hydrothermal treatment. The possible

mechanisms for converting Rambutan leaves into CQDs through microwave method

can involve several processes by using electromagnetic energy that emitted from

microwave irradiation. The electromagnetic energy will be absorbed by solvent

precursor, which is water for this experiment. Due to the energy from microwave

irradiation, water will cause the CQDs molecules to change the arrangement of its

carbon chains continuously and will produce kinetic energy that lead to generate heat

energy for the CQDs carbonization process[15].

 Figure 3. The physic characteristic of CQDs through microwave method from (A)
DRL-CQDs and (B) FRL-CQDs ; The emission of CQDs through microwave method
from (C) DRL-CQDs and (B) FRL-CQDs

Another Visual test using the UV laser from the excitation wavelength of 405 nm was

shown in Figure 3-C&D. The emission wavelength from both DRL-CQDs and FRL-

CQDs tended to emitted visible cyan to blue-green. However, DRL-CQD possess

brighter emission compared to others. Both sample have similar results with previous

literature by microwave treatment where emission wavelength from tea-CQDs [18]

emitted bright blue emission.

Uv-Vis characterization result.

Figure 4. shown the absorbance spectra of CQDs from each sample. The absorbance

spectra of the samples from both dried and fresh Rambutan leaves through different

method shown that there were absorptions from each of sample. All of the samples

contained CQDs based on the optical absorbance that were in the range of ultraviolet

wavelength (200−400 nm) and the intensity were decreased in the range of visible and
[1,19,20]
infrared wavelength . From the UV-visible spectroscopic analysis it was observed

that the absorption peak of DRL-CQDs from hydrothermal method is at 268.8 nm and

390 nm. These two peaks indicate the presence of π-π* transition of C=C bonds and the
[21]
n-π* transition of C=O bonds in CQDs, respectively , while the CQDs formed by

using fresh Rambutan leaves obtained single absorption peak at 298.78 nm which are

due to a π-π* transition of C=C bonds [23]. The other samples, DRL-CQDs and FRL-

CQDs through microwave treatment also assigned a single absorption peak at 300 nm

and 301.19 nm which is ascribed to the π-π* electronic transition of C=C [21]. The

difference surface structure from all of the samples might cause the absorption peak
shifted to the longer wavelength. In addition, the maximum absorption intensity in

absorption spectrum assigned the amount of CQDs formed.

Figure 4. UV-vis spectrum of CQDs

This experiment result showed that synthesis CQDs from all of samples was similar to

the previous literature that reported the UV-visible absorption spectrum of CQDs are

typically shown to have peak in ultraviolet region with a tail extending in visible region.

The absorption of CQDs is usually located in 230-300 nm is generally attributed to π-π*

transition of C=C and the peak/shoulder located around 310-500 nm is attributed to n-π*

transition of C=O[23,4,24,25,26].

Photoluminescenes characterization result.

Figure 5. shown the fluorescence spectra of CQDs from each sample. The wavelength

of the highest intensity peak from the fluorescence spectra of each sample are shown

below. The CQDs aqueous solution showed obvious cyan emission under UV light (405

nm). The fluorescence process that occurs in a particle in a medium will absorb

excitation light to be converted into fluorescent light emission, however, not all

absorbed light can be converted into emitted light, therefore the quantum yield

calculation will be considered as the effectiveness of the light conversion process of

absorbed excitation light into emission light. In this study, the highest QY obtained was

2.70% with the maximum emission peak at the excitation wavelength of 405 nm.

Table 1. Quantum Yield of each sample

DRL- FRL- DRL- FRL-

CQDs Material
Hydrothermal Hydrothermal Microwave Microwave
Quantum Yield 2,70 % 1,26 % 1,01 % 0,76 %

Briefly, the emission peak shifted to the shorter wavelength and its corresponding

fluorescence intensity decreased with for DRL-CQDs – hydrothermal, FRL-CQDs –

hydrothermal, DRL-CQDs – microwave, and FRL-CQDs – microwave, respectively.

The DRL-CQDs and FRL-CQDs from hydrothermal method exhibited a strongest

emission at 490 nm and 473.45 nm upon excitation at 405 nm, while the maximum

emission intensity of DRL-CQDs and FRL-CQDs from microwave method were

detected at 466 nm and 458 nm when excitation wavelength was 405 nm.

Figure 5. Fluorescense spectra of CQDs

The shift of the maximum emission peak towards the lower wavelength (blue-shift)

occur due to the difference in energy needed to make the transfer from the S1 energy
level to the S0 energy sub-level to the basic energy state level [27,28]. In addition, the band

gap energy obtained from the results of this study also varies between 3.51 eV - 2.52

eV. When the particle size gets smaller, the band gap of a particle will get bigger and
[29, 30]
require more energy to excite and de-excite electrons at lower wavelengths .

Whereas the difference in emission intensity from each sample is due to the difference

in the number of excited particles from each sample[34].

Table 2. Band gap energy of each sample

DRL- FRL- DRL- FRL-

CQDs Material
Hydrothermal Hydrothermal Microwave Microwave
Band Gap Energy 2,52 eV 2,98 eV 3,01 eV 3,51 eV

Another emission peak were found at 677 nm and 671 nm from DRL-CQDs and FRL-

CQDs from microwave, respectively. These peaks indicated the chlorophyll compounds

remaining in the samples[31]. However, the chlorophyll intensity of the samples were not

too high compare to the CDQs compound. The emission color emitted from each

samples corresponded to the wavelength range of 430 -590 nm at blue-yellow in color

spectrum[32]. The photoluminescenes-experiment result was resemble to the previous

literature, where maximum emission peak from leaves derived CQDs has a range of

wavelength at 405-500 nm with bright blue emission[16,17,4,26].

FT-IR characterisation result.

Figure 6. shown the FTIR spectra of CQDs from each sample. The FTIR spectrum

could be explained by various peaks obtained in the sample. The FTIR spectra of both
Rambutan leaves condition were recorded for comparison. The absorption peak of

CQDs for each sample, dried and fresh rambutan leaves through hydrothermal and

microwave method were recorded at 3332.96 cm -1 , 3333.61 cm-1 , 3328,42 cm-1 and

3323,62 cm-1 was assigned to –OH group. The absorption peak at 1635.38 cm -1 ,

1634.31 cm-1 , 1634.20 cm-1 , and 1635.42 cm-1 was assigned for C=O stretching for

each samples. Meanwhile, the other absorption peak at 665.91 cm -1, 604.10 cm-1 and

564,77 cm-1 were finger-print for DRL-CQDs - hydrothermal whereas peak at 661.70

cm-1 and 599,91 cm-1 were finger-print for FRL-CQDs - hydrothermal. For the DRL-

CQDs – microwave finger-print absorption peak showed at 657.78 cm -1, 603.91 cm-1

and 565,40 cm-1. While the absorption peak at 666.10 cm-1, 603.94 cm-1 and 561,61 cm-1

were observed as finger-print for FRL-CQDs - microwave. In the finger-print area there

are various absorptions due to various molecules interactions, so it’s difficult to

interpret the functional group contained in each sample in this area correctly [35].

This FTIR spectrum can be proved that all samples contained carbon dots, it is related to

Liu et al. 2007 studied about functional groups contained in the Cdots are O-H bonds

and N-H bonds in absorption bands 3100-3450 cm-1. In addition, there are other
functional groups in the absorption band 1600-1707 cm-1, namely C=O bond[36].

Figure 6. FT-IR spectra of CQDs from (A) DRL-CQDs - hydrotehrmal, (B) FRL-CQDs
– hydrothermal, (C) DRL-CQDs – microwave, and (D) FRL-CQDs – microwave
Cu2+ detection result.
Visual test for CQDs emission sensitivity to the increasing Cu 2+ ion concentration effect

was carried out to analyze the sensors ability of CQDs from various samples to heavy

metal ions. The fluorescence sensor mechanism occurs based on a decrease in

fluorescence intensity with the addition of an analyte called the quenching process [37].

Measurement of the fluorescence properties of the four CQDs samples is shown in

Figure 4.7. The figure below observed that Cu2+ can be detect by CQDs from all natural

samples. They were found to be effective for sensing and detection of Cu 2+ ions with

good selectivity and sensitivity. The emission intensity from each samples decrease

gradually as the Cu2+ ion concentration increased from 50 µM, 100 µM, 200 µM to 400

µM. The significant PL-Quenching occur after the addition of Cu 2+ ion. CQDs from

each sample has carboxyl and carbonyl atom on its surface. The efficient binding

affinity with vacant d-orbital of Cu2+ and carbonyl in CQDs can refer to its natural

selectivity in this sensing system. While the the -OH atoms donates electron pair to

2+
vacant d-orbital of Cu ions and non-radiative electron transfer will be occur. This

2+[23]
result the quenching process of CQDs in presence of Cu . Figure 4.7-D observed

the shifted emission peak to the red-shift area as its corresponding to the increasing the

Cu2+ ion concentration. It might be occur due to the bigger particle size change, because

particle size obtained is related to the obtained particular wavelength[26].

The CQD sensitivity can be measured by a very significant decrease in emission

intensity when the CQD responds to the analyte (Cu 2+). The result of this study showed

similar result as previous literature in which using CQDs as biosensor. The adding of

metal ion corresponding to the decreasing of CQDs emission intensity. The result
obtained also in accordance with research of (S. Liu, et al). They used grass as carbon

sources to synthesis CQDs as biosensor and reported that the sensitivity of CQDs as

detector can be tested by adding metal ion to the solutions. The results show that along

with the addition of Cu2+ ion concentration, the emission intensity tend to decrease

significantly, this proves that the CQDs synthesis obtained are very sensitive to the
[38]
presence of copper metal ions . (Yingshuai, et al) also reported that the highest

emission sensitivity obtained from the synthesis CQDs could be due to the high QY in
[26]
the sample . Based on the experiment, it can be seen that the CQDs from DRK -

hydrothermal shows the most sensitive behavior to the effect of the addition of heavy

metal copper, thus the CQDs can be used for further development as detection agent for

detecting a hazardous metal.

Figure 7. Fluorescence properties of CQDs as biosensor from (A) DRL-CQDs -

hydrothermal, (B) FRL-CQDs – hydrothermal, (C) DRL-CQDs – microwave, and (D)
FRL-CQDs – microwave
 Table 3. LOD of each CQDs sample

CQDs Material DRL FRL

LOD (µM)
Synthetic Method
Hydrothermal 123,67 346,12
Microwave 189,52 355
Based on Stern–Volmer equation for LoD measurement from Figure 8. below, the

result showed that LoD for each sample from DRL-CQDs – hydrothermal, FRL-CQDs

– hydrothermal, DRL-CQDs – microwave, and FRL-CQDs – microwave are 123,67

µM, 346,12 µM, 189,52 µM dan 355 µM, respectively as shown in the Table 1. The

LoD results obtained were relatively large due to the concentration range used was

large, but the results obtained showed that the results of the CQDs synthesis in this

study were very sensitive to detect the presence of Cu 2+ ions, so it is suitable to be

applied as a biosensor to detect the presence of copper metal.

 Figure 7. Selectivity investigation F0/F to fluorescence emission of CQDs from (A)
DRL-CQDs - hydrothermal, (B) FRL-CQDs – hydrothermal, (C) DRL-CQDs –
microwave, and (D) FRL-CQDs – microwave

Conclusion

We used Rambutan leaves as carbon sources to synthesize CQDs through one step-

hydrothermal and microwave method. Thess method has advantages of extremely low

cost, simple without any hazardous chemicals, and easy manipulation. The synthesized

light and dark brown CQDs solution emitted strong cyan fluorescence under the

irradiation of ultraviolet light with a wavelength of 405 nm. After the optimization of

preparing material conditions which is using dried and fresh Rambutan leaves and

characterization of CQDs, we found the best preparation material condition is the dried
leaves through hydrothermal method. It is known that the absorbance from dried

rambutan leaves from hydrothermal method has two absorption peak that observed the

π-π* and n-π electron transition which indicated to C=O and C=C bond compare to

others which is only have one absorption peak that indicate the π-π* electron transition

(C=C bond). The surface contains a large number of hydrophilic, carboxylic, and

carbonyl groups. Furthermore, the dried Rambutan leaves through hydrothermal

treatment has highest intensity compare to other sample which is the maximum

emission at 490 nm. Moreover, result obtained showed CQDs was found to be effective

for sensing and detection of Cu2+ ions with good selectivity and sensitivity. The results

obtained in this work provided a way to reduce costs for the practical application of

CQDs in the future.

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