Discover Materials

Review

A review of synthesis methods, and characterization techniques

of polymer nanocomposites for diverse applications
Shimelis Tamene Gobena1,2 · Abraham Debebe Woldeyonnes1

Received: 1 July 2024 / Accepted: 2 September 2024

© The Author(s) 2024  OPEN

Abstract
Polymer nanocomposites have become a quickly growing area of study, fueling the advancement of sophisticated
materials in recent years. Adding nanoparticles to a polymer matrix greatly improves the characteristics of the resulting
nanocomposites. These improvements play a crucial role in a wide range of applications, including dental restorations,
biosensors, food packaging, electronic devices, and various biomedical uses. This review offers a thorough examination
of various techniques for synthesizing polymer-based nanocomposites, such as melt intercalation, sol–gel processes,
in situ polymerization, and emulsion techniques. Moreover, it is essential to characterize these nanocomposites to com-
prehend their mechanical properties, structure, and morphology. Methods like atomic force microscopy (AFM), X-ray
diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) are widely utilized
for the examination of these attributes. The thermal properties of polymer nanocomposites are highly interesting, along
with their mechanical properties. Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA), and Fourier
Transform Infrared Spectroscopy (FTIR) are used to assess these thermal and chemical characteristics. In general, the
review seeks to summarize the methods of combining and analyzing polymer nanocomposites, giving a thorough insight
into how these processes enhance the improvement and refinement of materials for various industrial and medical uses.

* Shimelis Tamene Gobena, [email protected]; [email protected] | 1Department of Mechanical Engineering,

Addis Ababa Science and Technology University, P.O. Box 16417, Addis Ababa, Ethiopia. 2Artificial Intelligence and Robotic Center
of Excellence, Addis Ababa Science and Technology University, P.O. Box 16417, Addis Ababa, Ethiopia.

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Graphical Abstract

Keywords Nanomaterial · Polymers · Characterization · Synthesis techniques

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1 Introduction

Polymeric nanoparticles is prepared through dispersing performed polymers using different methods like, solvent
evaporation, nanoprecipitation, salting-out, and supercritical fluid technology [1]. Polymer matrices are widely used
due to their lightweight properties, ease of production and ductile nature. Polymer systems face some problems such
as modulus and strength are lower than metals and ceramics. The best practice to improve the properties of the poly-
mer system is the addition of particles such as platelets, whiskers and fibers to form a composite with the interacting
elements of the matrix and other materials. [2].
Polymer nanocomposite matrices consist primarily of a polymer matrix and a dispersive phase at the nanometric scale
in one dimension. Typically, incorporating fillers at a weight percentage of 10–40% substantially enhances the mechanical
properties of the resulting matrix [3 Combining nanomaterials that have a high aspect ratio and rigidity with a polymer
matrix enhances the performance of the polymer [3]. Various fillers can be used in nanocomposite matrices, including
metal nanoparticles, carbon nanotubes, silica, zinc oxide, calcium carbonate, and laminar silicate. This content aims to
explore the different synthesis methods for creating polymer-based nanocomposite matrices [1–3].

1.1 Polymer nanocomposite

Nanocomposite (NC) are define as solid and colloidal particles of macromolecular substances ranging in dimen-
sion 100 nm [1] There are several application areas which led to the investigation of different nanocomposite
[2]. Organic NPs, lipid-based NPs and metal-based NPs [2]. Synthetic materials and synthetic materials are used
for the preparation of polymeric NPs [3]. Polymers are used as synthetic materials due to the useful properties,
good biocompatibility, biodegradability, ease of preparation and design, chemical diversity, and attractive biologi-
cal properties [4]. Accordint to Moosa et al. [5] Most polymeric Nanocomposites (PNC) were recognized as biode-
gradable and biocompatible over the accomplished few decades [6].
They used to deliver drugs, proteins, peptides, and antigens also targeted to particular organ DNA transporters
in gene therapy [7]. Energy sectors, automobile industry, in aerospace and military industry are preferred area in
future [8]. Protein can help to synthesis polymers from, milk proteins and gelatin; polysaccharides such as starch,
chitosan and sodium alginate[9]; and synthetic polymers such as poly methyl methacrylate, poly(cyanoacrylate) PCA,
poly- caprolactone (PCL), poly (lactic acid)(PLA), poly (D, L-glycolic acid) (PGA),and their copolymer of poly (lactide-
co-glycolide) PLGA are used in preparing nanocomposite systems [10].

1.2 Classification of polymer nanocomposites

NPs are classified depending on their morphology, size and chemical properties. Shakeel et al. categorized Based on
physical and chemical characteristics, some of the well-known classes of NPs are [1, 11] carbon based nanoparticles(
NPs), metal based NPs, ceramics NPs, semiconductor, polymer NPs [1]

1.3 Classification based on the dimension of nanofillers

In recent literature, the classification of nanofillers has been discussed based on their dimensions. This paper reviews
the various types of nanofillers according to their applications. Zero-dimensional nanofillers, for example, possess
nano-scale dimensions in all directions and can be in the form of nanoparticles that are crystalline, amorphous,
ceramic, or metallic in nature[12, 13]. One-dimensional nanofillers having nano range dimension along just one direc-
tion such as nanowires and nanotubes[12].They usually have needle-like forms such as nanoplatelets, nanorods, nan-
oclays and nanosheets [14] with conductive nanocomposites and stretches based on alginate and silver nanow-
ires to create electronic devices. Two-dimensional nanofillers carbon nanotubes are the best possible examples [14].
It can also include nanofibers, nanorods and nanowhiskers [12] synthesized polyacrylamide/montmorillonite nano-
composites and studied their properties in solution [15]. Three-dimensional nanofillers have dimensions in the order
of nanometers in three dimensions [16].

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1.4 Classification based on the type of nanofillers

A) Metal Sulfide: Metal sulfide nanoparticles are believed to improve the stability of the obtained nanocomposite
compared to the polymer matrix [17]. Metal sulfides such as CdS, ZnS, are embedded in polymer materials [18,
19]. There can be many methods for creating such nanocomposites, but the most important is the hydrothermal and
thermal decomposition method [20] of synthesized zinc sulfide sodium carboxymethyl cellulose nanocomposite film
[15–18].
B) B). Metal hydroxide: These types of nanocomposites are well known for their flame retardant properties [21].
The main nanofillers used are magnesium and aluminum hydroxides, usually in the form of wires and fibers [21].
The polymer matrices used can be poly (vinyl chloride), elastomers, phenolic compounds and unsaturated polyesters
[22]. As the temperature increases, endothermic decomposition of metal hydroxides begins [23].They thus makes it
possible to separate heat treatment into materials. The support of such charges on the surface makes the barrier of
the ceramic or vitreous layer [14, 17, 21].
C) C). Metal Oxide: can be synthesized using different methods such as hydrothermal methods, sol gel methods, son-
ochemical approaches and coprecipitation methods. Examples of nanofillers include silica, ferric oxide, tita-
nium oxide and copper oxide [24]. synthesized an electrochromic material consisting of polyaniline-based nanofib-
ers covering nanorods of antimony-doped tin oxide and titanium oxide [4, 25].
D) Silicate: Silica powder is prepared with alcohol such as [26, 27] ethanol, ammonium hydroxide, water mixed with water
and hot air and then add different dispersions and dispersions [28]. After separating the parts of the dispersion and
silica synthesized for identification, residual silica expanded. It is treated with a silane coupling agent [26]. The clay
material is resistant to transport therefore the heating effect is not seen due to the coating [29]. Synthesized iron
oxide-polymer nanocomposite integrated with laminated magadite silicate using ion exchange and synthesis method
and used for oil recovery [28, 30].

1.5 Structural properties of polymer nanocomposite

In polymer nanocomposites, structure–property interactions are critical in determining how the inclusion of nanofillers
affects the overall performance of the material [31]. The distribution, size, shape, and interaction of nanofillers within
the polymer matrix significantly influence mechanical, thermal, and electrical properties [32]. At the nanoscale, the
increased surface area of fillers leads to enhanced interfacial interactions, which can improve the dispersion and bond-
ing between the fillers and the polymer [33]. These interactions affect properties such as tensile strength, modulus, and
impact resistance.

2 Synthesis of polymer nanocomposite:

Various methods can be employed for the synthesis of Nanomaterials, but these methods are broadly divided into two
main classes [11] as illustrated in the below Fig. 1.
Nanoparticle preparation methods can be divided into physical and chemical methods depending on whether chemi-
cal reactions are involved [34]. On the other hand, these systems can be divided into gas phase, liquid and solid phase [2]
depending on the conditions of the reaction system [35] The process of gas includes the process of gas heating (resistance
heating, high temperature heating, plasma heating, electric heating, laser heating, electric heating, vacuum or sputtering)
[36]. Liquid fraction nanoparticle synthesis methods mainly include precipitation, hydrolysis, spraying, thermal melt-
ing process (high temperature and high pressure), melting evaporation pyrolysis, redox (ambient pressure), l emulsion,
chemical synthesis by radiation and Sol–gel processing. Solidification methods include combustion, solid state reactions,
annealing, pickling and grinding [37].

2.1 Synthesis of polymer nanocomposite by sol gel

The term “sol–gel” refers to a process that includes two reaction phases: sol and gel. In this context, the “sol” is
a colloidal suspension in which a solid is dispersed in a liquid. A "gel" is a cohesive network that forms between
these processes. The sol–gel method is widely used to produce solids from small particles at low temperatures [7].
In this process, the most important step is the conversion of the precursors into the colloidal through hydrolysis and

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Fig. 1  synthetic methods for

Nanoparticles top-down and
bottom-up system [11]

Fig. 2  The process of polym-

erization in Sol–gel Method
[39]

condensation reaction [33]. In this process, particles or fillers are dispersed in a monomer solution (called sol) that
emerges from the layers of the particle. These results in the formation of an interactive network of polymers and nan-
oparticles (called gel) [34]. Therefore, the polymer contributes to the nucleation and growth of nanomaterials [38].
This method is similar to the surface method [35] prepared by chitosan and salicylaldehyde in the presence of TiO2
nanofillers to form a nanocomposite membrane [4] The recovery of metals, excess water, solvents, heat and the use of
complex substances or catalysts are the main reactions [3]. Whether it is used or not depends on the chemical nature
of the metal atom and the strong resistance of the alkoxide group. The electrophilic nature of the metal atom and
its ability to increase the coordination rate are the main factors [36]. As Dmitry Bokov et.al said in their experimental
research [37], compatibility with polymers and polymerization filix, which shows the possibility of nanoparticle for-
mation in the presence of organic molecules, shown in Figs. 2, 3 and 4.
Advantage of the sol gel synthesis methods are uniform nanoparticle dispersion, control particle size, low tem-
perature versatility and can control porosity [40]. However some it is complex process to control in aggregation also
scalability and post synthesis process is issue [31].

2.2 In situ polymerization

The process works on the principle of the absorption of the monomer solution by the platelets as they respond [34].
This is followed by the polymerization of the monomer under the influence of heat, initiators or UV light. There-
fore, the formation of exfoliated nanocomposites or intercalated nanocomposites takes place [39]. In situ template
synthesis is another method in which the size of the platelets is controlled as a polymer matrix [40] and the plate-
lets move in a high fluid such that the nucleation of the platelets is under the control of the polymer chains that
enter the do them [41]. However, this method has the disadvantage of increasing the decomposition of polymer
chains at high temperatures [42].

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Fig. 3  Scheme of synthesis of sol–gel method: a films synthesized from colloidal sol and b powder synthesized from gel [40]

Fig. 4  An overview of the types of processes that can be done with the sol–gel method and the products of each process [40]

2.3 Intercalation method

The general communication process involves the dispersion of nanoplatelets as nanomaterials in a polymer matrix
[40]. It is well known that the incorporation of clay (nanomaterials) into polymer matrices improves properties such
as hardness, resistance and fire resistance. Intercalation is a top-down method that requires modification of the
nanoplatelet surface for the diffusion of platelet-like nanofillers in the polymer matrix [26] An additional strain occurs
when the polymer chains diffuse into the gallery space of the layered structure. Nanoplatelets can be individu-
ally dispersed by chemical and mechanical methods [43]. The chemical process is a process, in which the nano-
particles are dispersed in the monomer, then the polymerization reaction takes place, then the nanoplatelets are
dispersed in the polymer, followed by another polymerization process [2]. Nanoplatelets react with the monomer
solution and polymer formation occurs between the assembled sheets through the polymerization process [44].
The repair method is to inject the polymer into the nanoplatelets directly by mixing the solution [45]. The polymer
is dissolved in the coating and the nanoplatelets pieces react with the solvent. The two solutions are mixed and the

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Fig. 5  mechanisms for green synthesis (extracellular) of NPs using microbes

Fig. 6  Nanoparticle preparation techniques [47]

polymer chains from the solution enter the nanoplatelets cavity and remove the solvent [46] as shown in Fig. 6. The
relationship between the working surfaces is very important in the effectiveness of the intercalation method, as
they affect the connection and the performance of the intercalated. Poor social interaction can lead to problems such
as temporary or negative separation, undermining the value of the relationship.[41, 42].

2.4 Green synthesis

The biological and green synthesis of nanomaterials offers a superior alternative to traditional chemical and physical
methods. This approach, embedded in a green chemistry framework, leverages nanoscale attributes to create materi-
als that have garnered significant interest for their potential applications across various sectors. This research explores
the increasing importance of nanocomposites produced using eco-friendly, green technologies. The shift toward green
synthesis aligns with the global push for environmentally sustainable practices, reducing reliance on conventional, harsh
synthetic techniques.
The application of ’green’ materials and nanoparticles derived from bio components is poised to become widespread
across various industries, including pharmaceuticals, environmental management, food, and cosmetics[43]. These materi-
als offer a sustainable alternative to conventional materials, addressing the growing demand for eco-friendly solutions
as it illustrated on Fig. 5. Green synthesis methods utilize natural polymers such as cellulose and bacterial-derived gellan

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gum to create innovative composite materials. Cellulose-based films provide biodegradability and mechanical strength,
making them ideal for packaging, wound dressings, and edible films. Gellan gum, a polysaccharide produced by bac-
teria, enhances the composite’s stability and biocompatibility, which is beneficial for drug delivery systems and tissue
engineering [44]. The incorporation of such bio components not only reduces environmental impact but also improves
the functionality of nanomaterials, offering enhanced properties such as biodegradability, non-toxicity, and improved
mechanical performance [41, 45]. These advancements in green synthesis are driven by scientific innovations and align
with the global movement towards sustainable industrial practices.

2.5 Electro spinning

Electro spinning is a widely used technique for synthesizing polymer nanocomposite fibers, involving the formation of
fibers from a polymer solution under an electric field [46]. This method allows precise control over fiber diameter, mor-
phology, and composition, resulting in nanocomposites with improved mechanical, thermal, and electrical properties.
These fibers are used in diverse applications such as filtration, catalysis, energy storage, and biomedical fields like tissue
engineering and drug delivery. The technique’s ability to disperse nanoparticles uniformly and create multifunctional
materials makes it valuable for developing advanced materials with specific functionalities. The NP preparation process
from organic and inorganic is shown in following Fig. 6 and the PNC synthesis techniques and material were stated in
Table 1.

3 Applications of polymer‑based nanocomposites

Nanocomposite material can be applied in many areas, such as manufacturing of, medical equipment’s, cancer therapy,
prosthesis materials, military device, electromechanical, in automobile, and etc. In the Medical area, the use of these
materials has been gaining prominence attention in recent years [57–59].

3.1 Dental restoration

The incorporation of nanoparticles into dental composites has led to improved clinical applications. The application
of nanoparticles in these materials can improve mechanical properties, surface smoothness and polishing and reduce
polymerization shrinkage [60–62]. From a mechanical point of view, the incorporation of nanoparticles into dental
composites can improve many mechanical properties, such as wear resistance, elastic modulus, flexural strength, frac-
ture toughness and fracture toughness [63, 64]. The use of nanotechnology and polymeric materials include types of
nanofillers, many studies have shown the ability of these fillers to increase the strength and reduce the hardness of the
final restoration [65, 66]. The purpose of nanocomposites in dental restoration is to mimic the composition of dental
tissue. Human teeth are mainly composed of two highly mineralized tissues, dentin and enamel. These tissues have an
inorganic component composed mainly of nanoparticles of natural calcium such as hydroxyapatites and calcosperites
[51–53].

3.2 Polymer nanocomposites in electronic devices

Carbon nanotubes and graphene-based polymer nanocomposites have shown excellent electrical properties and can
be used for the fabrication of electronic devices [49–51, 67]. Some polymers such as polyaniline, polyacetylene, polypyr-
role [56, 68] can be used to make electro conductive materials [10, 34]. The electrical and mechanical properties of these
polymers can be improved by enhancing them with nanomaterials such as graphene [50, 69]. Graphene exhibits highly
conductive properties due to its large surface area and strong π-π interactions [70]. It also has special features such
as high flexibility, high electrical conductivity, light weight, etc. These properties enable the application of polymer-based
nanocomposites in electronic devices [49–52].

3.3 Tissue engineering and drug delivery

This process involves creating new tissue by combining parent cells into structures. Optimizing the balance of these struc-
tures is important to ensure cells receive adequate nutrients and efficiently remove metabolic waste. Fabrication of

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Table 1  the synthesis techniques for polymer nanocomposite are summarizing in following table
Polymers Components Precursors Methods References

Epoxy SiO2 and ­TiO2 TEOS and TIP Combination of sol–gel and in situ polymerization [48]
Polyaniline (PANI) TiO2 APS Ex-situ and in-situ chemical oxidation polymerization [49]
Epoxy SiO2 HCl thermal treatment [5]
Polymethyl methacrylate (PMMA) PLA AIBN (azophloxine) Optical filtering and thermal polymerization [9, 50]
Polyacrylonitrile TiO2 and Ag NaOH Sol gel solution [51, 52]
Propylene Al2O3,MoO3 and Fe2O3 TIP Chemical vapor decomposition (CVD) [53, 54]
Adenine-containing polyimide Nitrogen (N) Cellulose and lignin In situ polymerization [10, 13]
Tetragonal zirconia polycrystals ZrO2 Zirconium oxychloride octahydrate (ZrOCl2 Sol gel preparation, Hydrothermal and coprecipitation [54, 55]
Epoxy Polyaniline Ammonium persulfate (APS) oxidative chemical polymerization (CVD) [4, 56]
Epoxy TiO2 Ticl4 Direct precipitation [37]
Resin OMMT Acetyltrimethylammonium chloride (MMT-CTAC) Hydrothermal and sol gel preparation [7, 26]
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micro engineered hydrogels using top down and bottom up methods [29]. The bottom up approach uses the micro-
scale characterization of relatively large hydrogel particles, while the top-down approach is used to create small building
blocks for assembly [20]. The low functional capacity and highly liquid nature of hydrogels pose significant challenges
in vivo and in vitro drug delivery systems [38, 53]. The delivery facilities of therapists at their target sites can be improved
for efficient delivery. For example, a tyrosine-based silica-polycarbonate xerogel nanocomposite has been developed to
facilitate targeted drug delivery [71]. Nanoparticles are also used for targeted drug delivery to enhance poor drug absorp-
tion at disease sites [72].

3.4 Polymer nanocomposites in biosensing

Recently, materials scientists have focused on electrochemical immune-sensing applications involving quantum dots
and polymer nanocomposites with metal (Ag/Au) components [73]. In one study, graphene oxide nano sheet-polyaniline
nanowire-CdSe quantum dot (GO-PANI-CdSe) were designed for the detection of interleukin-6 [29]. The synthesized NCs
have combined the properties such as, high electrical conductivity of Polyaniline with electrochemical luminescence of
CdSe and large surface area of graphene oxide [74, 75].
PANI-AuNP PWEs (PANIAuNP-modified paper working electrodes) had shown Biosensing applications for the detection
of two tumor markers, α-fetoprotein and carcinoembryonic antigen, in human serum [76] have synthesized an immune
sensor based upon Grp-AuNP-poly-DPB-AuNP-IL composite film for analyzing microcystinLR. This sensor enhances the
electron transfer of Fe (CN)6 3-/4- to the electrode. They can substitute antibodies due to their greater stability and high
target-specific affinity compared to the antibodies to the desired target site [76]. The AuNP-PS-aptamer-poly TTBA-AuNP-
GCE is an example of an aptamer sensor designed for detecting daunomycin [29]. For the detection of aflatoxin M1,
Fe3O4-PANI-IDE (interdigitated electrodes modified with Fe3O4-incorporated PANI films) was employed. The aptamer
were immobilized through glutaraldehyde cross-linking [77]. For instance, poly (pyrrole-NTA)/Cu2 + /HisTBA-Pt, which
consists of poly(pyrrole-nitrilotriacetic acid) complexes with Cu + ions and histidine-tagged thrombin adaptor immo-
bilized on a platinum surface, has been utilized for the quantitative detection of thrombin [1]. This is just one example
among many where polymer nanocomposites serve as aptamer sensors.

3.5 Polymer nanocomposites in the packaging industry

Polymer nanocomposites (NPCs) find application in the beverage industry for packaging finished products. Among the
polymer matrices used to develop nanocomposite films for packaging are polypropylene (PP), nylon, polyethylene (PE),
and polyethylene terephthalate (PET) [78]. Nanocomposites are highly versatile for packaging applications because
they offer enhanced properties like thermal, dimensional, and chemical stability, as well as heat resistance. They also
provide high mechanical strength and excellent optical clarity, thanks to the nanoscale size of the particles used [79].
Such types of packaging materials also possess gas, oxygen, and water barrier properties [80]. Polymer matrices enhance
the thermodynamic stability of metal containing nanoparticles [81]. Multilayer nanocomposite materials are used for
rigid packaging.

4 Polymer nanocomposite Characterization techniques

Different dynamic methods are available to study the degree of intercalation/exfoliation and their corresponding effect
on the properties of nanocomposites [82]. The physical appearance of the polymers (color, shape, size, visible holes or
cracks on the polymer surface and/or biofilm formation) was recorded before and after processing [83]. Characterization
of nanocomposite materials is important to understand/analyze the different properties of polymer nanocomposites
[39] the nature of the dispersion of the filler in the polymer matrix and its structure or composition depending on the
processing method used [84], effect of filler surface modification on filler dispersion and composite properties [85].
The interaction of the modification with the polymer chain, including the chemical reaction between the two, the
change in the process and the morphology and the resulting materials [79], and besides that, research. of different mate-
rials to determine the application strength of nanocomposites[64–66] is the key finding in nanocomposites.

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Fig. 7  a A schematic diagram of an AFM system [86]. b Scheme of the optical detection system [88]. c sample interaction profile of Force
tapping model [88]

4.1 Atomic force microscopic (AFM)

Recently, AFM is absolutely the most useful and powerful tool to characterize sample surface at a nanoscale: unlike
electronic microscopy or scanning tunneling microscopy, it does not require previous treatment of a sample, such as
metallization [86]. In Fig. 7 important PNCs characterization mechanism are stated. Atomic Force Microscopy (AFM),
is characterization techniques, which allows for characterizing topographic, adhesive, friction, roughness, and nano-
mechanical features by a raster-scanning sample surface [86] Furthermore, AFM permits obtaining information about
the mechanical properties of the investigated material [87]. Through the analysis of the tip sample contact function,
the parameter like adhesion viscoelasticity modulus and shear can be found. In the last few years significant progress
has been made by applying imaging capabilities edge protection and numerical methods for multi frequency meas-
urements, adding new AFM features such as amplitude peak [72, 73]. In addition, in an exciting research, Garcia and
Herruzo discussed the development of five different types of multi-frequency power microscopy, focusing on applica-
tions in proteins, nanostructures and cells, opening the way for spatial integration, composition and periodic capacity.
environmental factors and access to resources are not considered in classical microscopies [88]. The solid line shows the
laser beam for the natural cantilever position without bending, while the dashed lines mark the width reflected by the
cantilever bending vertically in the lateral view [84].
Under a driving sinusoidal wave, the scanner sets a synchronization window. The peak force point is extracted in about
half a period. The tip gradually approaches the measured surface with a stable zero force baseline before the snap-in
state of tip-sample contact. After reaching the peak force, the tip retracts and is off the surface at the adhesion peak state
[37, 88] sample interaction profile in the Peak Force tapping mode [88] is shown in Fig. 8.

4.2 X‑ray diffraction (XRD):

X-ray diffraction was used to analyze the changes that occur in the clay due to the dissolution [89]. XRD is a good method
to study interstice of clay particle due to its simplicity [90] and availability [57, 67]. XRD analysis shows peaks for clays
and organoclays due to their high resolution structure [49]. This peak conform platelet separation or spacing in clay
structure [82, 91]. Genix & Oberdisse, [92] Fractional scattering of X-rays or neutrons is due to the spatial variation of long-
range density at the nanoscale. By measuring the scattered energy (or more specifically the cross section per unit sample
volume) as a function of the vector q, one can draw conclusions about the nanostructure [52, 93]. Figure 9 shows the
distribution pattern of NP aggregates.

4.3 Transmission electron microscopy (TEM)

TEM is widely used to investigate the dispersion of polymer-layered silicate nanocomposites (PLSN). However, image anal-
ysis techniques can be used to determine the dispersion of TEM images [94]. Samyn et al., [94] extracted different param-
eters that provide detailed information and also provide a good description of the microstructure. The average thickness,

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Fig. 8  According to Stan & King, 2020 [88] Bimodal AFM images of a a ternary blend polymer surface made of polypropylene (PP), polyeth-
ylene (PE), and polystyrene (PS) regions and b a homogeneous ultra-high molecular weight polyethylene (UHMWPE) surface. c Histogram of
the CR frequencies (third eigenmode of the Cantilever) over the surfaces in (a, b). d Conversion between the measured CR frequencies and
elastic moduli with UHMWPE used as a reference with a Young’s modulus around 1.3 GPa

Fig. 9  a Illustration of scatter-

ing typical of NP aggregates. b
Example of chain scattering in
polymer melts as encountered
during the dissolution of latex
beads. Data are taken from
reference [92]

Fig. 10  The image shows the collected data processing image analysis: the particle curved length (L), thickness (t), and the interparticular
distance in the direction parallel to that of the lengths of the tactoids (ek)and perpendicular to the latter orientation (adopted from Samyn
et al., [94]

length and cross-sectional area of ​​each class of tactoids can be measured as well as their size and the average dis-
tance between two adjacent tactoids [95]. Therefore, the absence of a maximum number does not mean that the elimina-
tion is completed completely, but that they are pressed due to a large gap [96]. Scanning electron microscopy (TEM) pro-
vides the most specific method to investigate the state of clay dissolution, because this method allows imaging of objects
at the nanoscale [82]. TEM technique to visualize the quality of nanoparticles [54]. The researcher found the distribution
of nanoparticles in some small agglomerates of the matrix [82].
TEM pictures of the PA6 nanocomposite are presented in Fig. 10, by Stan & King, 2020 [88]. These pictures show that
clay platelets are individually and evenly dispersed in the polymeric matrix. The dispersion achieved in the PBT is illus-
trated by the TEM pictures shown in Fig. 11.

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Fig. 11  a TEM pictures of the

PA6 nanocomposite (Stan and
King) [88], b TEM picture of
the PBT nanocomposite (Stan
and King) [88]

4.4 Scanning electron microscopy (SEM)

Scanning electron microscopy (SEM) techniques are commonly used to investigate surface morphology of polymers
and to detect growth of microorganisms on polymers during preparation [78]. SEM uses focused beam of electrons
which produces images of a sample by scanning it. The polishing of surface is done to make it conductive [83].

4.5 Differential scanning calorimetry (DSC)

DSC is one of the most commonly used methods to study the Brownian transition of primary polymers and their com-
posites [97]. The transition temperature (Tg) is one of the most important properties of polymer electrolytes related to
electrochemical properties [97]. It is influenced by the structure of the polymer chain, crystallinity, viscosity, polymer
interactions or polarity and molecular weight of polymers [60]. This transition value is defined by the value of the glass
transition temperature (Tg). It is defined as the transition temperature of any system from solid phase to rubbery/vis-
cous phase. Below Tg, there is no ion migration or the chain is not activated [81]. Above Tg, there is a dramatic change
in the internal properties (density, specific heat, mechanical modulus, mechanical absorption, dielectric and acoustic
compatibility) of the polymer that favors rapid movement or low viscosity [36]. Differential scanning calorimetry
(DSC) is used to measure Tg and it also provides the melting and crystallinity of the material used [81]. A low value of
Tg indicates the flexibility of the polymer matrix [82]. The main strategy to reduce the Tg value is to change the struc-
ture of the polymer chain and break the covalent bonds between the polymer chains. This can be achieved by add-
ing nanofillers, plasticizers, nano-clay, etc [72–74].

4.6 Thermogravimetric analysis (TGA)

TGA is also the most important tool to compare the thermal stability of the different organically modified fillers [83].
So, the thermal stability is investigated by TGA to check the safety window of a polymer electrolyte [84].
As different materials have different decomposition temperature ranges and for long-term cycle stability of all
materials must lie beyond the decomposition range [85]. The important factor affecting the thermal performance

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Table 2  Summary of characterization of polymer nanocomposite depend on recent literature

Characterization techniques Properties analyzed References

Gravimetric % Weight loss [82]

Tensile strength Mechanical strength, modulus, and elongation [88, 98]
XRD/WAXRD Crystallinity, interlayer spacing and dispersion degree of Nano scale fillers, kinetics of the poly- [99, 100]
mer melt intercalation process
DSC Crystallization and melting properties [26, 51]
TGA​ Thermal Stability(Ts), [34, 55]
DMTA Thermal Transitions [77, 101]
Oxygen gas permeability Oxygen gas transmission rates [28]
POM Surface characteristics [26, 102]
UV Visible spectrometry Transmittance of UV and visible light [13]
Fluorescence microscopy Enumeration and viability of bacterial cells [14]
AFM Particle size and distribution, surface morphology and microstructure, degree of crystallization [19, 103, 104]
FTIR Chemical analysis, crystallization and orientation of polymer, interfacial interactions [9, 105]
NMR Chemical analysis [106]
GPC/SEC Average molecular weights [2]
SEM Surface morphology, microstructure like grain size, imperfection [107, 108]
TEM Internal structure and morphology of nanoscale fillers in composites [89, 109, 110]
Clear–zone Resistance or susceptibility of plastics to microbial degradation [111]
Pour plate or Streak plate Enumeration and isolation of degrading microorganisms [14, 112]
Molecular Detection identification of degrading microorganisms [77, 113]

of materials is the environment in which the TGA analysis is carried out. [41] The thermal stability of the fillers was
better in the case of the nitrogen atmosphere as compared to the air atmosphere. [1, 48]. The summary of NPCs
characterization techniques were assessed with the properties material and shown in Table 2.

5 Conclusion

The nanocomposite polymer matrices are highly efficient for their multidimensional perspective and application. Recently
PNCs are applicable in different manufacturing industries for different propose like as dental restoration in medicine,
automobile, drug-delivering, and in the food packing industry. There in this paper, the characterization techniques
and synthesis method are reviewed. Nanocomposite polymer matrices are very potential for future use, but there are
still many improvements to bring. Generally, the optimization of physicochemical functions such as charging density,
hydrophobicity, porosity, and mechanical and thermal stability of polymer nanocomposites is important. Also, the aggre-
gation of nanofillers within the polymer matrix is a major issue to ensure the uniform distribution of nanofillers across
polymer nanocomposites. Future research in the synthesis and application of polymer nanocomposites should focus
on three key areas: reducing the carbon footprint, leveraging artificial intelligence (AI), and utilizing 3D printing. First,
developing environmentally friendly synthesis methods that minimize energy consumption and reduce waste is crucial
for decreasing the carbon footprint. Research should explore alternative, sustainable materials and processes that offer
the same or better performance as traditional methods. Second, AI has the potential to revolutionize the design and
optimization of polymer nanocomposites by providing predictive models for material behavior and guiding synthesis
processes. This can lead to more efficient use of resources and shorter development cycles. Finally, 3D printing technol-
ogy can significantly enhance the manufacturing of polymer nanocomposites by enabling precise control over material
properties and structure, reducing material waste, and customizing applications to meet specific needs. By integrating
these advancements, researchers can develop more sustainable, efficient, and innovative polymer nanocomposite solu-
tions for a wide range of industries.

Author contributions 1. Shimelis Tamene Gobena: Corrsponding Author 2. Abraham Debebe Woldeyonnes: co-Author.

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Data availability No datasets were generated or analysed during the current study.

Declarations
Competing interests The authors declare no competing interests.

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the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this licence, visit http://​creat​iveco​
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