Characterization techniques:
Nanomaterials are used in various fields because of their variation in properties with size and
shape. We can measure properties like size distribution, degree of aggregation, surface charge
and surface area, etc. by studding different parameters in the characterization of nanoparticles.
Characterization is mainly the study of materials features such as its composition, structure, and
various properties like physical, chemical, electrical, magnetic, etc. [1] Some of the
characterization techniques are given by:
Scanning electron microscopy (SEM):
SEM analyzes the morphology of nanomaterials and provides detailed surface imaging [2]. It
utilizes a beam of accelerated electrons and electromagnetic lenses, achieving magnification up
to 100,000× and enhanced depth of field. The high-energy electrons are focused on the solid
sample's surface, generating various signals that convey information about the topographical
details and atomic composition [3]. SEM gives the morphology, shape of nanoparticles,
agglomeration and dispersion of nanoparticles [4, 5]. Some of the compositional
characterizations are carried out by energy dispersion X-rays spectroscopy (EDX) attached with
SEM.
Transmission electron Microscopy (TEM):
TEM is the most effective method for nanomaterial characterization, offering spatial resolution
from the atomic level (1–100 nm) to the micrometer level. It provides direct images and
chemical information about nanomaterials. TEM offers higher resolution than SEM as it utilizes
powerful electron beams [2]. ]. TEM gives the morphology and shape of nanoparticles,
agglomeration, core shell localization and dispersion of nanoparticles [4, 6]. TEM is the only
method to visualize the localization of magnetite, confirming magnetite is truly inside the core
shell or merely attached to the surface [6]. The HR-TEM allows the visualization of Lattice
fringes (the actual rows of atom).
X-ray Diffraction (XRD):
XRD is a widely used analytical technique for determining the size, phase, and orientation of
crystals. It also describes the type of nanoparticle [6]. XRD is based on constructive interference
of monochromatic X-rays and crystalline sample. Constructive interference only occurs when the
path difference between waves reflected from adjacent planes is an integer multiple of the X-ray
wavelength [7]. This relationship is expressed by Bragg’s Law:
nλ=2 dsinθ
Where, n is the order of diffraction, λ is the wavelength of the X-rays, d is the interplanar
spacing between atoms and θ is the angle of incident also called Bragg’s angle [8].
XRD is frequently be used for average crystallite size. As size of particles become smaller the
peaks become broader [9]. These peaks are estimated by Scherrer equation:
Kλ
D=
βcosθ
Where, D is the size of crystal domains, K is a dimensionless space factor and β is the line
broadening at half the maximum intensity in radian [10]. It is important to keep it in notes that
the crystallite size measured by Scherrer equation may be smaller than the actual size observed
in SEM and TEM, if particle is composed of multiple crystals [10].
UV-visible spectroscopy and photoluminescence spectroscopy (PL):
In absorption spectroscopy such as UV–vis, the transition of electrons from the ground state to
an excited state is measured, while in photoluminescence spectroscopy, the transition of
electrons from the excited state to the ground state is measured [11]. UV–vis spectroscopy uses
visible and UV light to measure the absorption or reflectance of a sample. In photoluminescence
spectroscopy, usually UV light is used to excite the electron and then measure the luminescence
or fluorescence properties of a sample [12]. Nanoparticles have unique optical properties that are
sensitive to the size, shape, concentration, agglomeration state, and refractive index near the
nanoparticle surface, which makes UV-Vis a valuable tool for identifying, characterizing, and
studying nanomaterials. Deuterium and tungsten lamps are used to provide illumination across
the ultraviolet, visible and near-infrared electromagnetic spectrum.
UV-visible spectroscopy follows Beer – Lambert law which states that the concentration of the
sample is directly proportional to the absorbance A.
A=log 10 ( )
Io
I
=ϵcl
Where, A is absorbance, ϵ is the Molar absorptivity, c is the concentration of the nanoparticles
and l is the Path length of the cuvette. UV-visible Spectroscopy serves as a vital tool for
electronic structure of nanoparticles [13].
Zeta potential:
FTIR spectroscopy:
References:
1. Dam, Samudrapom. (2024, October 24). An Overview of Nanomaterial Characterization
Methods. AZoNano. Retrieved on May 04, 2026 from
[Link]
2. Singh, A., et al. (2024). Nanomaterial Characterization Techniques. Futuristic Trends in
Chemical Material Sciences & Nano Technology. DOI:
10.58532/V3BECS13P1CH2, [Link]
NOMATERIAL_CHARACTERIZATION_TECHNIQUES
3. Thaher, Y., Chandrasekaran, B., Panchu, SJ. (2020). The Importance of Nano-materials
Characterization Techniques. Integrative Nanomedicine for New Therapies. DOI:
10.1007/978-3-030-36260-7_2, [Link]
36260-7_2
4. Li, Z., Zhao, S., & Zhang, Y. (2023). An overview of synthesis and structural regulation
of magnetic nanomaterials prepared by chemical coprecipitation. Metals, 13(1), 152.
[Link]
5. Scurtu, R., Iacovita, C., & Lucaciu, C. M. (2021). Magnetite-silica core/shell
nanostructures: From surface functionalization towards biomedical applications—A
review. Applied Sciences, 11(22), 11075. [Link]
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Synthesis, characterization, and biomedical applications. Magnetochemistry, 8(10), 120.
[Link]
7. Technology Networks. (2025). X-Ray Diffraction (XRD) – XRD Principle, XRD Analysis
and Applications. [Link]
diffraction-xrd-xrd-principle-xrd-analysis-and-applications-404260
8. BYJU'S. (2021). Braggs Law - Derivation, Formula, and Applications.
[Link]
9. Scribd. (2020). X-Ray Diffraction Principles and Methods.
[Link]
10. Wikipedia. (2026). Scherrer equation. [Link]
11. Skoog, D. A., Holler, F. J., & Crouch, S. R. (Eds.). (2017). Principles of instrumental
analysis (7th ed.). Cengage Learning.
12. Patel, S., Patel, P., Undre, S. B., Pandya, S. R., Singh, M., & Bakshi, S. (2016). DNA
binding and dispersion activities of titanium dioxide nanoparticles with UV/vis
spectrophotometry, fluorescence spectroscopy and physicochemical analysis at
physiological temperature. Journal of Molecular Liquids, 213, 304–311.
[Link]
13. Habibi, M. H., et al. (2021). Electronic and optical characterization of doped spinel
structures. Nanomaterials, 11(4), 892. [Link]
14.