Synthesis of Silver Nanoparticles through Orange

Peel Powder for Antibacterial Composite Filler

Applications
Rathinavel Subbiah (  rathinavelaero59@gmail.com )
Nehru Institute of Engineering and Technology https://orcid.org/0000-0002-2549-5893
S. S. Saravanakumar
Kamaraj College of Engineering and Technology

Research Article

Keywords: Orange Peel Powder (OPP), Antibacterial property, Silver nanoparticles, Filler material, Thermal
property

Posted Date: June 16th, 2021

DOI: https://doi.org/10.21203/rs.3.rs-239984/v1

License:   This work is licensed under a Creative Commons Attribution 4.0 International License.
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Synthesis of Silver Nanoparticles through Orange Peel Powder for Antibacterial Composite
Filler Applications

S. RATHINAVEL 1* , S. S. SARAVANAKUMAR 2

1
Assistant Professor Department of Aeronautical Engineering, Nehru Institute of Engineering

and Technology, Coimbatore 641 105, Tamil Nadu, India.

2
Associate Professor Department of Mechanical Engineering, Kamaraj College of Engineering

and Technology, Virudhunagar 626 001, Tamil Nadu, India.

*Corresponding author: S. RATHINAVEL (rathinavelaero59@gmail.com)

1
Abstract

Environmental concerns and the positive aspects of biowaste materials gained the attention of researchers to use

them as filler materials in fabricating of green composites along with polymer matrices, but most of them are not

suitable for extensive applications in high thermal applications. In most of the natural particulate materials are not

having the ability to fight against pathogens. To overcome such barriers, a modification of biowaste - Orange Peel

Powder (OPP) by the generation of silver nanoparticles (AgNPs) is prepared with the one-step hydrothermal

process. The modified Orange Peel Powder (MOPP), is then characterized by FESEM, EDX, FT-IR, XRD, and

Thermal analyses. The presence of AgNPs in the MOPP is confirmed through FESEM & EDX analysis. FT-IR

spectral analysis pronounced the non mutate functional groups in MOPP as compared with OPP. The generation of

AgNPs in MOPP is confirmed through the XRD peaks of reflection planes at (1,1,1), (2,0,0), (2,2,0) & (3,1,1).

Thermal Analysis results of TGA and DSC show the MOPP has increased thermal stability up to 363°C.

Antibacterial test against Gram-negative and Gram-positive bacteria for OPP & MOPP shows the inclusion of Ag

strongly objects the pathogens. Eventually, the MOPP can be utilized as filler material along with the polymer

matrix in high thermal as well as antibacterial composite filler applications.

Graphical Abstract

Keywords

Orange Peel Powder (OPP), Antibacterial property, Silver nanoparticles, Filler material, Thermal property

2
Introduction

Majority of the agricultural wastes as well as municipal solid waste left unused and create problems to the

environment and municipal solid waste management in countries like India and European countries[1]. Studies

revealed that agricultural wastes of 200 million tons were generated in India alone and 998 million tons globally[2].

In that organic fruit waste of Cítricos del Andévalo Orange Juice processing company located in Spain contributes

400 tons every day even though they can be reused[3]. Organic fruits like Orange posses 50-60% of their total

weight as waste in forms of peels, seeds and membrane residue. Orange peels contain 17.5% of cellulose, 8.5% of

hemicellulose and Pectin[4]. The cognate chemical composition materials were reported by the researchers for

various applications like Ocimum sanctum leaves with silver nanoparticles to form films for packaging

application[5], Chitosan in plated with silver nanoparticles for the application of the natural rubber latex[6], Acacia

leucophloea fibers for the design of lightweight materials[7], Tamarind leaf with silver nanoparticles used for the

antibacterial textile materials[8], and Pennisetum purpureum grass formulated with copper nanoparticles for the

application of dressing materials in the medical field[9]. With the above incentive, Orange Peels in the Powder form

can be utilized for packaging applications in addition to the polymers matrices as a filler. To improve its utilization

in large scope it can be modified by adding silver nanoparticles to involve the same in high thermal applications..

Silver nanoparticles (AgNPs) were generated from the aqueous silver nitrate solution (AgNO3) and they possess

good chemical as well as thermal properties[10],[29]. From the literatures, the lack of compatability analyse of the

biowaste materials are found, to utilize as a filler material especially along with silver nano particles. The anti

bacterial activity of the natural waste materials can be improved with the addition of AgNPs in order to improve its

utilization as a filler material along with polymer matrix for the application of packaging films. By this inclusion of

AgNPs the thermal properties of this biowaste materials can also be improved and also the utilization in the high

thermal applications like packing foods to improve their shelf life.

In this investigation, OPP has been modified with silver nanoparticles by the hydrothermal process and the modified

OPP (MOPP) is characterized and suggested that the MOPP can be used as a filler material for the high thermal

green composite applications.

Materials And Methods

Materials

3
Orange Peel Powder (OPP) was procured from MG Naturals, Chennai, Tamil Nadu with the size of less than 50 µm.

The ultrapure grade of silver nitrate (AgNO3) was purchased from Modern Scientific company, Madurai, Tamil

Nadu and used as procured.

Preparation of Modified Orange Peel Powder (MOPP)

The preparation of MOPP was done by the procedure described elsewhere[11] [30]. Briefly, The 3grams of OPP

was added to the 50ml of 5mM aqueous solution of AgNO3 and stirred with a magnetic stirrer for a period of

24hours at the temperature of 80°C. The modification of OPP can be observed by coloration change from pale

yellow to dark brown. Then the MOPP separated and dried in the oven for 3hrs at the temperature of 100°C.

Characterization of Nano composite Bio film

Microscopic Analysis (FESEM)

The morphological study of AgNPs in MOPP had been evaluated by the images of FESEM and EDX spectra

through Carl Zeiss- Sigma with Gemini column at a magnification of 1µm and operated at 20kV. The experiment is

to analysis the distribution of silver nanoparticles in the MOPP

FTIR Analysis

The functional groups in the MOPP & OPP are determined through the FT-IR spectrum recorded by Perkin-Elmer

783. The spectrophotometer in the range of 4000 cm-1 to 500 cm-1 with 4 cm-1 resolution and 45 scans for both the

case using KBr pellets.

X-ray Diffraction Analysis (XRD)

To record the x-ray diffractogram of MOPP and OPP, to analyse the materials present as well as plane of reflection

in both OPP and MOPP the EXPERT-PRO diffractometer system was used with the generator setting of 30MA,

40KV. The anode material was Cu and the position in the range of 2θ = 10° to 80°. The reflection planes of AgNPs

presented in the MOPP had been calculated by,

Bragg's law

𝜆
d=
2𝑠𝑖𝑛Ɵ

and

4
 𝑎
d= (1)
√ℎ2 +𝑘 2 +𝑙2

Thermogravimetric Analysis (TGA)

The thermogravimetric analysis for MOPP & OPP was carried out on NETZSCH STA 2500 Regulus instrument

with the temperature range of 30°C to 550°C at 10 °C/ min heating rate at an nitrogen atmosphere with a flow rate of

20ml/min. From the TGA, thermal stability of OPP and MOPP were obtained. To obtain the derivative form of

thermo gram the differentials of primary thermogram was calculated by central finite difference method [12] i.e.,

DTG = (𝑊𝑡 + ∆𝑡 − 𝑊𝑡 − ∆𝑡)/2∆𝑡 (2)

where,

Wt+Δt & Wt-Δt are residual weight samples at t+Δt and t-Δt time,

and Δt is time for reading sample residual weight

Kinetic activation Energy

The Broido's kinetics equation was used to determine the Kinetic activation energy through[13] [31],

1 𝐸 1
𝐼𝑛 [𝐼𝑛 ( )] = − ( 𝑎) [( ) + 𝑘] (3)
𝑦 𝑅 𝑇

Where,

R- Universal gas constant (8.314 J/mol.K); T-Temperature in K; Ea-Kinetic activation energy

K-reaction rate constant

𝑊𝑡
y= Where, Wt- Weight at Time 'T'; Wo- Weight at Initial
𝑊𝑜

1
The Broido's Plot between 𝐼𝑛 [𝐼𝑛 ( )] & (1/T) used to determine the kinetic activation energy.
𝑦

Differential Scanning Calorimetry (DSC)

DSC was performed to find glass transition tempertaure of both OPP & MOPP, on NETZSCH STA 2500 Regulus

instrument at a heating rate of 10 K/ min under Nitrogen atmosphere by following ASTM E-967 ASTM 2008a and

ASTM E-968 ASTM2008b standards[10],[32].

Result and Discussion

Microscopic Analysis (SEM) & EDX Spectra

5
Figure 1(a) shows the Scanning Electron Microscopic image of MOPP. Figure 1(b) represents the EDX spectra

recorded from the SEM image.

Fig. 1 (a) SEM Image of MOPP (b) EDX Spectra of MOPP

In Figure 1(a), the spherical shape particles indicates the in-situ generates AgNPs which are marked in

arrow heads. From Figure 1(b) the EDX spectra peak corresponding to 2.98 KeV~3 KeV value in the X axis

confirms the presence of Ag in the MOPP along with C and O. The presence of C and O is confirmed through the

peaks at 0.2 and 0.3 KeV respectively[19],[33].

FTIR Analysis

The FTIR spectra ranges from 4000 cm -1 to 500 cm-1 for MOPP and OPP are shown in Figure 2 to observe the

chemical groups present in them. In this observation, the spectra of MOPP and OPP showed a broad band between

3500 cm-1 to 3100 cm-1 assigned to O-H stretching (hydroxyl groups). The peak at 2992 cm -1 wave number

recognized to -C-H- stretching vibration of alkenes[14]. The absorption bands at 1741cm-1 and 1622 cm-1

represented C=O stretching present in hemicelluloses [7] and -C=C- stretching respectively. The 1521 cm -1 arise due

to the C=C ring stretching (Aromatic group). 1438 cm -1 peak observed due to carbonyl stretching raise in lignin[15].

The bands at finger print region, 1016 cm -1 clarified the C-O-C vibrational stretching of polysaccharides[11] and

838 cm-1 confirmed the presence of glucosidic (β) linkages between hemicelluloses and cellulose sugar units[7]. The

C-OH bending in cellulose observed through peak at 598 cm -1[16],[34]. From the Figure 2 it is conspicuous that

there is slight shift in the peaks of MOPP as compared to the OPP such as 2924 cm-1 to 2992 cm-1 , 1743 cm-1 to

1741 cm-1 , 1612 cm-1 to 1622 cm-1 and 1016 cm-1 to 1018 cm-1 likewise the intensity of those peaks lowered in the

MOPP due to reduction of silver ions to AgNPs (Ag + to Ag) but it clearly evident that the minor shift in peaks

6
does not affected the functional groups present in the OPP during synthesis of AgNPs. The shift in the peaks as well

as reduction in the intensity of the peaks are due to the involvement of functional groups in the synthesis of AgNPs.

The results of FTIR spectral also revealed that no chemical interaction between AgNPs and OPP during preparation

of MOPP[17].

Fig. 2 FTIR spectra of OPP & MOPP

X-ray Diffraction Analysis (XRD)

X-ray diffractogram of MOPP and OPP are presented in Figure 3. It is evident that the presence of two common

peaks at 2θ = 14.1° and 21.5°, which are due to the reflection planes (1 0 0) of cellulose-I present in the OPP &

MOPP[5]. These peaks were most likely to be exhibited in natural materials. In MOPP X-ray diffractogram in

addition to above two peaks, peaks at 2θ = 37.9°, 44.4°, 64.3° & 77.2° were observed. With the help of Bragg's law

represented as equation (1), reflection planes of those peaks were found to be (1,1,1), (2,0,0), (2,2,0) & (3,1,1) of

7
AgNPs respectively[15]. These peaks and planes of reflections are well-matched with the ICDD (International

Centre for Diffraction Data) PDF (Powder Diffraction File) 04-0783 for Ag[20].. Thus the MOPP has the silver

nano particles in it (AgNPs).

Fig. 3 X-ray Diffractogram of OPP & MOPP

Thermogravimetric Analysis (TGA)

TGA analysis is for analyzing the thermal stability based on the weight loss of the material with the increase of

temperature. DTG curves are derived using equation (2). Figure 4(a) and (b) showed the TGA and DTG thermo

grams of MOPP and OPP. Three stages of thermal degradations observed in both the powders, clearly through DTG

curves. The initial degradation found to be identical for both MOPP & OPP at 100°C with weight loss of 4.27% for

8
MOPP and 6.22% for OPP with the effect of moisture evaporation. The intermediate degradation observed at 232°C

for OPP & 246°C for MOPP with the higher weight loss by MOPP with 7.96% where as OPP exhibited 5.87% due

to the degradation of pectin, hemi cellulose and links of cellulose [18]. The final degradation between 250°C to

400°C, the higher mass reduction of the MOPP & OPP observed because of complete degradation of cellulose. The

mass loss observed at 400°C for MOPP is 48.7% and for OPP is 54.1%. There is a change in the point of inflection

observed in MOPP as compared to OPP due to the inclusion of thermally stable AgNPs. The MOPP thermally stable

up to 363°C where as thermal stability of OPP is 357°C. The residual mass of MOPP observed as 35% but OPP

exhibited 24% of residual mass at 548°C. The higher residual masses of MOPP is due to the inclusion of high

thermal withstanding capacity AgNPs.

Fig. 4 (a)TG - Curves of OPP & MOPP (b) DTG thermo grams of MOPP & OPP

Kinetic Activation Energy

It is the minimum energy required to start the degradation of the samples and are calculated from the equation (3),

the activation energy for the thermal degradation of the MOPP & OPP in the temperature region of 200°C to 375°C

1
was evaluated[21]. Figure 5 (a) and (b) shows the plot between 𝐼𝑛 [𝐼𝑛 ( )] and (1/T) for the OPP& MOPP. The
𝑦

slope value of the generated straight line related to the activation energy in order to understand the thermal

degradation of both the materials[22],[23]. The activation energy (Ea) of OPP is 71.50 KJ/mol which is increased to

9
91.10 KJ/mol in the case of MOPP. The aforementioned increase in activation energy is due to the effect of AgNPs

present in the MOPP.

Fig. 5 Broido's Plot of (a) OPP & (b) MOPP

Differential Scanning Calorimetry (DSC)

DSC curves of the OPP & MOPP are presented in the Figure 6. DSC curve of OPP has a broad endothermic curve

initially up to 100°C due to the decomposition of water present in them. OPP exhibits endothermic curves shows a

two melting point peaks (Tm1 & Tm2). Tm1 corresponds to the degradation of hemicelluloses at around 230°C and

the Tm2 showed the degradation of cellulose at 347°C[24]. Glass transition temperature (Tg) of the OPP is around

80°C. Moreover exothermic cures of MOPP showed the enhanced melting points Tm1 & Tm2 in correspondence to

the degradation of hemicelluloses and cellulose[25],[26]. The Tm1 of MOPP observed at 250°C and Tm 2 at 362°C.

Likewise the glass transition temperature of MOPP is improved to 102°C. The results ascribed the generated AgNPs

improves the thermal behavior of the MOPP.

10
 Fig. 6 DSC thermo grams of OPP & MOPP

Antibacterial Test

Both OPP and MOPP were tested against P. aeruginosa, E.Coli (Gram-negative) and S. aureu, S. oralis (Gram-

positive) bacteria. The antibacterial activities of the OPP and MOPP are assessed based on the zone of inhibition in

the agar plate showed in Figure 7. The large zone of inhibition relates to the strong antibacterial activity of the

samples[27],[28]. The inhibition zones of OPP and MOPP against pathogens are listed in Table 1. The OPP powder

posses a partial inhibition zone in the range of 13.5 mm to 17.4mm whereas the MOPP showed the strong inhibition

zones from 37.4mm to 39.0mm of diameter because of the silver nanoparticles present in them. This implied that the

MOPP has the ability against pathogens due to the antibacterial activity of AgNPs nature.

11
Fig. 7 Zone of inhibition formed by OPP(A1) and MOPP(A2) against (a) E. coli, (b) P. aeruginosa, (c) S. aureus and
(d) S. oralis

Diameter of inhibition zone (mm)

Sample
Gram-negative Gram-positive
(Code)
E. Coli P. aeroginosa S. aureus S. oralis
OPP (A1) 15.5±0.5 17.4±0.4 13.5±0.5 15.6±0.7
MOPP (A2) 38±0 37.4±0.8 38.5±0.3 39.0±0.1

Table 1 Antibacterial activity of OPP and MOPP

Conclusions

Owing to stretch the applications of biowaste filler materials, the modification of the OPP was done with the

hydrothermal process for the in-situ generation of silver nanoparticles(AgNPs). The MOPP was characterized using

SEM, EDX, FT-IR, XRD and Thermal Analysis. The presence of silver nanoparticles in MOPP was identified

through SEM and EDX. Further, no change in the functional groups of MOPP was observed during the generation

12
of AgNPs by FT-IR analysis. The XRD result confirmed the presence Ag by the peaks mentioned by the ICDD. The

generated AgNPs improved the thermal behavior of the MOPP by increased thermal stability up to 363°C and

Kinetic activation energy of 91.10 KJ/mol. Likewise, the glass transition temperature is also improved to 102°C.

The zone of clearance produced against gram- negative and gram-positive bacteria by MOPP represents the strong

antibacterial activity as compare to OPP. With the above results the MOPP can be act as a filler material along with

the polymer matrices for the fabrications of green composites in high thermal as well as antibacterial applications.

Acknowledgements

Authors are thankful to managements of both Kamaraj College of Engineering & Technology, Virudhunagar 626

001, Tamil Nadu, India, and Nehru Institute of Engineering & Technology, Coimbatore-641 105, Tamil Nadu, India

for their support and encouragement.

Conflict of Interest

There is no conflict of interest among the authors.

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