SYNTHESIS OF SILVER NANOPARTICLES USING

DISMODIUM ELLIGANCE PLANT EXTRACT AND ITS

CONJUGATION WITH POLYPYRROLE

First step involves reduction of metal ions and nucleation of reduce metal. This step is

known as activation phase. In 2nd step the small adjacent nanoparticles spontaneously coalesce

into particles of a larger size (direct formation of nanoparticles by means of heterogeneous

nucleation and growth, and further metal ion reduction; a process referred to as Ostwald

ripening), which is accompanied by an increase in the thermodynamic stability of nanoparticles.

This step is called growth phase. The 3rd step is termination phase which gives the final shape of

nanoparticles [25, 26].

There are also some other factors which affect the formation of metal ions into

nanoparticles. These factors include reaction mixture pH, incubation temperature, reaction time,

concentration, and electrochemical potential of a metal ion [4, 27-29].

Synthesis of silver nanoparticles

Synthesis by physical methods

There are many physical approaches but most important among them are evaporation-

condensation and laser ablation. Different nanoparticles like silver, gold, lead sulfide, cadmium

sulfide, and fullerene have been synthesized by using evaporation-condensation method.

Physical methods have advantages over chemical methods because of absence of solvent

contamination in prepared thin films and also nanoparticles distribution is uniform. Physical
method has some disadvantages in synthesizing nanoparticles using tube furnace at atmospheric

pressure, for example tube furnace occupies a large space, consumes a great amount of energy

while raising the environmental temperature around the source material, and requires a great deal

of time to achieve thermal stability. Further tube furnace requires power consumption more than

several kilowatts and a preheating time of several tens of minutes to reach a stable operating

temperature [30, 31].

Nanoparticles could also be synthesized using a small ceramic heater with a local heating

source. The evaporated vapor cools down at suitable rapid rate because in comparison with

temperature of tube furnace, the temperature gradient in vicinity of heater surface is very steep.

This gives formation of nanoparticles in high concentration. This physical method can be useful

as a nanoparticle generator for long-term experiments for inhalation toxicity studies, and as a

calibration device for nanoparticle measurement equipment [32].

Silver nanoparticles can also be synthesized by laser ablation of metallic bulk materials in

solution [33-37]. The ablation efficiency and the characteristics of produced nanosilver particles

depend upon many factors such as the wavelength of the laser impinging the metallic target, the

duration of the laser pulses (in the femto-, pico- and nanosecond regime), the laser fluence, the

ablation time duration and the effective liquid medium, with or without the presence of

surfactants [38-41].

Synthesis by chemical methods

Chemical reduction of sliver metal ions by organic and inorganic reducing agents is most

commonly used method to synthesize silver nanoparticles. There were different reducing agents

such as sodium citrate, ascorbate, sodium borohydride (NaBH4), elemental hydrogen, polyol
process, Tollens reagent, N, N-dimethylformamide (DMF), and poly (ethylene glycol)-block

Copolymers were used for reduction of silver ions (Ag+) in aqueous or non-aqueous solutions.

These reducing agents reduced silver ions (Ag+) and give the formation of metallic silver (Ag0),

which was then followed by agglomeration into oligomeric clusters. These clusters eventually

lead to formation of metallic colloidal silver particles [42-44].

Dodecanethiol capped silver nanoparticles were prepared using Brust procedure [45],

based on a phase transfer of an Au3+ complex from aqueous to organic phase in a two-phase

liquid-liquid system, followed by a reduction with sodium borohydride in the presence of

dodecanethiol as a stabilizing agent, binding onto the nanoparticles surfaces, thereby avoiding

their aggregation and making them soluble in certain solvents. It was reported that small changes

in synthetic factors gives interesting modifications in nanoparticle structure, average size, size

distribution width, stability and self-assembly patterns [46].

Hyperbranched poly(methylene bisacrylamide aminoethyl piperazine) was used with

terminal dimethylamine groups (HPAMAM-N(CH3)2) to give colloids of silver. The amide

moieties, piperazine rings, tertiary amine groups and the hyper-branched structure in HPAMAM-

N(CH3)2 were found important due to its stabilizing and reducing abilities [47].

UV-initiated photoreduction is another easy and simple method to synthesize silver

nanoparticles in the presence of citrate, polyvinylpyrrolidone, poly(acrylic acid), and collagen.

Silver nanoparticles were prepared by photoreduction of silver nitrate in layered inorganic

laponite clay suspensions which act as a stabilizing agent for preventing nanoparticles from

aggregation. These nanoparticles were studied as a function of UV irradiation time. When these

particles were irradiated under UV for 3 h, bimodal size distribution and relatively large silver

nanoparticles were obtained. When further irradiation was performed silver nanoparticles were
disintegrated into smaller sizes with a single distribution mode until a relatively stable size and

size distribution was obtained [48].

Silver nanoparticles (nanosphere, nanowire, and dendrite) were also prepared by an ultraviolet

irradiation photoreduction technique at room temperature using poly(vinylalcohol) (as protecting

and stabilizing agent). Concentration of both poly(vinylalcohol) and silver nitrate played

important role in the growth of the nanorods and dendrites [49].

Nano-sized silver particles with an average size of 8 nm were synthesized by

photoinduced reduction using poly(styrene sulfonate)/poly(allylamine hydrochloride)

polyelectrolyte capsules as microreactors [50]. Moreover, it was demonstrated that photoinduced

method could be used for converting silver nanospheres into triangular silver nanocrystals

(nanoprisms) with desired edge lengths in the range of 30-120 nm [51]. Growth of these particles

was controlled by using dual-beam illumination of nanoparticles. Citrate and poly(styrene

sulfonate) were used as stabilizing agents. Silver nanoparticles were also prepared by a very fast

reduction of Ag+ by -aminoalkyl radicals generated from hydrogen abstraction toward an

aliphatic amine by the excited triplet state of 2-substituted thioxanthone series

(TXOCH2COO and TXSCH2COO). This reaction leads to the conversion of silver

ions to metallic silver [52]. Silver nanoparticles were also synthesized by several irradiation

methods. Silver nanoparticles of well-defined shape and size distribution were prepared by laser

irradiation of an aqueous solution of silver salt and surfactant [53].

Nanoparticles were also prepared from benzophenone by using laser in a photo-

sensitization synthetic method. Low laser powers at short irradiation times produced silver

nanoparticles of approximately 20 nm, and an increased irradiation power produced

nanoparticles of approximately 5 nm. Silver nanoparticles were also synthesized by using laser
and mercury lamp as a light source [54]. The photo-sensitized growth of silver nanoparticles was

performed using thiophene (sensitizing dye) and silver nanoparticle formation by illumination of

Ag(NH3)+ in ethanol [55].

A simple one-step method called tollens method was used to synthesize silver

nanoparticles of controllable size. That green synthesis technique involved the reduction of

Ag(NH3)2+ (as a Tollens reagent) by an aldehyde [56]. In the modified Tollens procedure, silver

ions were reduced by saccharides in the presence of ammonia, which yields silver nanoparticle

films (50-200 nm), silver hydrosols (20-50 nm) and silver nanoparticles of different shapes. The

concentration of ammonia and nature of reducing agent plays important role in controlling size

and shape of silver nanoparticles.

Silver, gold, palladium, and platinum nanoparticles could be prepared at room

temperature, by simply mixing the corresponding metal ions with reduced polyoxometalates

which act as reducing and stabilizing agents. Polyoxometalates were soluble in water and had the

capability of undergoing stepwise, multielectron redox reactions without disturbing their

structure. It was reported that silver nanoparticles could be produced by illuminating a deaerated

solution of polyoxometalate/S/Ag+ (polyoxometalate: [PW12O40] 3, [SiW12O40] 4- ; S:propan-2-ol

or 2,4-dichlorophenol) [57]. Furthermore it was also reported the green chemistry-type one-step

synthesis and stabilization of silver nanostructures with MoVMoVI mixed-valence

polyoxometalates in water at room temperature [58].

Synthesis by biological methods

In recent years, silver nanoparticles of desired morphology and size prepared by green

chemistry method, becomes major focus for researchers in which natural reducing, stabilizing

and capping agents were used. Biological methods can be used to synthesize silver nanoparticles
without the use of any harsh, toxic and expensive chemical substances [59-62]. The mostly used

organisms in green synthesis of silver nanoparticles are discussed below.

Synthesis of silver nanoparticles using bacteria

Highly stable silver nanoparticles of 40 nm size could be synthesized by bioreduction of aqueous

silver ions with a culture supernatant of nonpathogenic bacterium, Bacillus licheniformis [63].

Moreover, bacterium Bacillus licheniformis were used to synthesize well dispersed silver

nanocrystal of size 50 nm [63]. Rapid biosynthesis of metallic nanoparticles of silver was

reported using the reduction of aqueous Ag+ ions by culture supernatants of Klebsiella

pneumonia, E. coli, and Enterobacter cloacae (Enterobacteriacae) [64]. The preparation process

was very fast and silver nanoparticles were synthesized within 5 minutes of silver ions coming in

contact with the cell filtrate. It seems that nitroreductase enzymes might be responsible for

bioreduction of silver ions.

Synthesis of silver nanoparticles using fungi

Silver nanoparticles could be synthesized extracellularly using Fusarium oxysporum, with no

evidence of flocculation of the particles even a month after the reaction [65]. Proteins stabilizing

silver nanoparticles might be responsible for the long-term stability of silver nanoparticles. The

morphology of nanoparticles observed in micrographs was generally spherical and occasionally

triangular shapes.

Stable silver nanoparticles were prepared by using Aspergillus flavus [66]. These

nanoparticles were stable in water for more than 3 months with no aggregation because of

surface binding of stabilizing materials secreted by the fungus [67]. Extracellular biosynthesis of

silver nanoparticles using Aspergillus fumigatus was also investigated. TEM results showed

well-dispersed silver nanoparticles (5-25 nm) with variable shapes. Most of them were spherical
in nature with some others having occasionally triangular shapes [68]. Extracellular filtrate of

Cladosporium cladosporioides biomass was used to synthesize silver nanoparticles [69]. It was

reported that proteins, organic acids and polysaccharides released by C. cladosporioides were

responsible for formation of spherical crystalline silver nanoparticles.

It was also reported that penicillium sp. J3 isolated from soil was able to produce silver

nanoparticles [70]. The bioreduction of silver ions occurred on the surface of the cells and

proteins might play a critical role in formation and stabilization of the synthesized nanoparticles.

Synthesis of silver nanoparticles using plants

Camellia sinensis (green tea) extract was used as a reducing and stabilizing agent for the

biosynthesis of silver nanoparticles in an aqueous solution in ambient conditions [71]. It was

reported that when the amount of C. sinensis extract was increased, the resulted nanoparticles

were slightly larger and more spherical. Phenolic acid type biomolecules (e.g., caffeine and

theophylline) present in the C. sinensis extract seemed to be responsible for the formation and

stabilization of silver nanoparticles. Black tea leaf extract was used for the synthesis of silver

nanoparticles. These nanoparticles were stable and had different shapes, such as spheres,

trapezoids, prisms, and rods. Polyphenols and flavonoids seemed to be responsible for the

biosynthesis of these nanoparticles [72].

High density of extremely stable silver nanoparticles (16-40 nm) were synthesized by

challenging silver ions with Datura metel (Solanaceae) leaf extract [73]. The leaf extracts of this

plant contains biomolecules, including alkaloids, proteins/enzymes, amino acids, alcoholic

compounds, and polysaccharides which could be used as reductant to react with silver ions, and

therefore used as scaffolds to direct the formation of silver nanoparticles in the solution. Stable

silver nanoparticles with average particle size ranging from 15 to 500 nm could be synthesized
extracellularly from Pinus desiflora, Diospyros kaki, Ginko biloba, Magnolia kobus and Platanus

orientalis leaf broths. It was noticed that M. kobus and D. kaki leaf broths, the synthesis rate and

final conversion to silver nanoparticles was faster, when the reaction temperature was increased.

But the average particle sizes produced by D. kaki leaf broth decreased from 50 nm to 16 nm,

when temperature was increased from 25 C to 95 C. It was also concluded that only 11 min

was required for more than 90% conversion at the reaction temperature of 95 C using M. kobus

leaf broth [74].

Silver ions could be reduced to silver nanoparticles of different shapes by using leaf

extracts from the aquatic medicinal plant, Nelumbo nucifera (Nymphaeaceae). These synthesized

nanoparticles showed larvicidal activities against malaria (Anopheles subpictus) and filariasis

(Culex quinquefasciatus) vectors [75]. Sorbus aucuparia leaf extract were used to biosynthesized

silver nanoparticles within 15 min. These nanoparticles were found stable for more than 3

months. The sorbate ion in the leaf extract of S. aucuparia seemed to be responsible for the

stability of silver nanoparticles [76].

Synthesis of polypyrrole-sillver nanocomposites

Silver and gold nanoparticles have been studied extensively due to their optical, electrochemical,

and electronic properties [7779]. During the synthesis of these nanoparticles, one should also

care about their agglomeration. To get rid of agglomeration surface coating is required. Many

stabilizing species have been studied including molecules with carboxylic acids, thiol groups,

inorganic materials, conventional polymers, and conducting polymers [8086]. To provide

stabilization against agglomeration, conducting polymers were used because they increase

electrical and electrochemical properties, improved conductivity, robustness, stability and

electrocatalytic activity [87, 88].

Among all metal-conducting polymer nanocomposites, polypyrrole (PPy)-silver nanoparticles

comes out to be very interesting material because it is environmental friendly and have high

conductivity and can easily be obtained [89-91]. PPy shows well characterized electrochromic

behavior due to the tunable nature of highest occupied molecular orbital and the lowest

unoccupied molecular orbital, which allows for the modulation of its optical and electrical

properties [88].

PPy-Agnanop nanocomposites could be synthesized by different chemical and electrochemical

procedures. PPy-Agnanop nanocomposites were synthesized by in situ chemical polymerization

through a redox reaction between pyrrole and silver nitrate [86]. PPy-Agnanop nanocomposites

were also synthesized at the interface of water and ionic liquid using one-step UV-induced

polymerization [92].
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