Table of Contents

Introduction .................................................................................................................................................. 1
Experimental Procedure .............................................................................................................................. 2
Synthesis Procedure of Carbon Dots ....................................................................................................... 2
Synthesis Procedure of MnO
2
-Carbon dots Composites......................................................................... 2
Results and Discussion ................................................................................................................................. 2
SEM characterization of carbon dots obtained ........................................................................................... 3
SEM images of carbon dots at 140C at different magnifications .......................................................... 3
SEM images of carbon dots at 180C at different magnifications .......................................................... 4
SEM images of carbon dots(less concentrated) at 200C at different magnifications .......................... 4
SEM images of carbon dots (highly concentrated) at 200C at different magnifications ...................... 5
SEM characterization of Composites ........................................................................................................... 6
SEM characterization of MnO
2
-Cabon dots (200C) Composites ............................................................ 6




Under Graduate Project 13-14 Report
Synthesis of Carbon Dots and
MnO2-Carbon Composites
Submitted by Nidhi Sahu
Introduction
Carbon Dots can be a used in place of traditional semiconductor quantum dots and applied to
future nanodevices, because of their advantages of water solubility, chemical inertness, low
toxicity, preferable biocompatibility, easy functionalization, and valuable photoluminescence.
There are various methods for the preparation of C-dots, including etching with larger carbon
materials, such as laser ablation, electrochemical oxidation, thermal oxidation, microwave
irradiation, hot injection, and pyrolysis. However, the previously reported methods for the
preparation of C-dots have several limitations, such as limited spectral efficiency, low product
yield, lack of size control, and the use of toxic chemicals or high temperature for experiments.
Consideration of preserving a green environment, preventing increasing global warming, and
ensuring sustainable and renewable sources of energy must be brought toward the preparation
of the C-dots.
A simple and facile one-pot synthesis of fluorescent carbon dots from lemon waste peels was
performed using the hydrothermal carbonization method at three temperatures
(140
0
C, 180
0
C, 200
0
C).
Hydrothermal carbonization could be an effective method due to its simple experimental setup,
which avoids the need of strongly toxic chemicals or high temperature. Mainly, water is used as
the reaction medium for the conversion of biomass, where the bulk and/or nano-sized carbon
materials are provided under mild experimental conditions. An environmentally friendly feature
of the hydrothermal carbonization method is the absence of either a strong acid or an organic
reagent. The present preparation of carbon particles in an aqueous medium has the advantage
of being considerably cheaper than conventional methods and absolutely green
The main purpose of this study is to confirm the formation of carbon particles from the
carbohydrate at the molecular level and to find efficient promotions to environmentally low-
load systems. The carbonization and functionalization occur through dehydration of the lemon
peels, which leads to the formation of fluorescent carbon particles with nanosize.
MnO
2
@colloid carbon spheres nanocomposites with tunable interior architecture have
been synthesized by a facile and cost-effective strategy at room temperature. Manganese
oxides were attractive due to their high theoretical specific capacitance, low cost and
environmental friendliness. Yet, the poor electrical conductivity and low specific area of
manganese oxide electrodes hampered the emersion of capacity. The electrochemical
properties of MnO
2
were mainly dependent on their sizes, structures and crystallinity.



Experimental Procedure

Synthesis Procedure of Carbon Dots
Lemon waste peels were collected, first washed in water and dried in sunlight, followed
by oven-drying at 100C for 10 h for carbonization.
5 g of the pretreated orange waste peels were kept in 100 mL of an aqueous 0.25 M
H
2
SO
4
solution for 15 min for oxidation and rinsed with water, followed by filtering.
The peels are then kept in an oven for drying at 100C for 4 hrs.
The obtained lemon peels were then mixed with 150 mL of a sodium hypochlorite
solution at room temperature for 4 hrs. to bleach all the colored material
The peels are then washed with distilled water until the pH of washed water reached 7.
The oxidized lemon peels (in 62.5 mL of water) were placed in a Teflon-lined autoclave
and kept at 140C for 12 h
The autoclave was allowed to cool down naturally, and the obtained brown solution was
washed with dichloromethane to remove the unreacted organic moieties.
The aqueous solution was centrifuged at 10000 rpm for 30 min to separate the solvent
from the mixture and finally dried at 100C until all the solution is dried and solid
particles are obtained.
The procedure is then repeated for two other hydrothermal temperatures (180C &
200C)
The yield is different for different temperatures
Synthesis Procedure of MnO
2
-Carbon dots Composites
40 mg of prepared carbon dots at 200C were dissolved in 160 ml of distilled water.
A solution of 20mM KMnO
4
(126.4 gm. KMnO
4
in 40 ml of water) is prepared.
A solution of 50mM H
2
SO
4
(1.8 ml H
2
SO
4
in 4.6 ml distilled water) is prepared.
All the solutions prepared are mixed together and kept at stirring for 4 hrs. at 40C.
The precipitates then obtained are washed with Water and then with Ethanol for 2-3
times and dried in vacuum.

Results and Discussion
The yield of the C-dots calculated from weight of raw material obtained is different for
different temperatures
Yield at 140C 4.51% (0.2256 g of 5 g lemon peels)
Yield at 180C 5.15% (0.2575 g of 5 g lemon peels)
Yield at 200C 9.15% (0.4574 g of 5 g lemon peels)

The weight of the composites obtained after drying in vacuum is 40.5 mg which is
approximately equal to the weight of the carbon dots used.
The prepared hydrothermal carbons were amorphous in nature.
The produced C-dots were readily soluble in water to form a stable, yellowish, and
transparent aqueous solution without precipitation for months

SEM characterization of carbon dots obtained

SEM images of carbon dots at 140C at different magnifications



The SEM image of the carbon
dots obtained at 140C shows flat surface
characteristics and no dots.
The reason may be less
hydrothermal temperature that is used.

SEM images of carbon dots at 180C at different magnifications


SEM images of carbon dots(less concentrated) at 200C at different magnifications





SEM images of carbon dots (highly concentrated) at 200C at different magnifications


















The SEM images were obtained at different magnifications. The carbon dots cannot be
seen clearly because the particles got agglomerate while preparing the SEM sample, as
the image shows, the image at less magnification shows some particles while in high
magnification it can be clearly seen that agglomeration has happened.




SEM characterization of Composites

SEM characterization of MnO
2
-Cabon dots (200C) Composites










The SEM images show carbon dots covered with MnO
2
fibers
The SEM images obtained shows carbon dots with MnO
2
fibers all over its surface and
around the gaps.
These extra fibers are obtained because of more Reaction time.