Classification of Nanomaterials

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Synthesis of nanomaterials using various top-down and bottom-up

approaches, inﬂuencing factors, advantages, and disadvantages: A review
Article in Advances in Colloid and Interface Science · December 2021

DOI: 10.1016/j.cis.2021.102597
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Advances in Colloid and Interface Science 300 (2022) 102597
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Advances in Colloid and Interface Science

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Historical Perspective
Synthesis of nanomaterials using various top-down and bottom-up

approaches, influencing factors, advantages, and disadvantages: A review
Namra Abid a, Aqib Muhammad Khan b, Sara Shujait a, Kainat Chaudhary a,
Muhammad Ikram c, *, Muhammad Imran d, Junaid Haider e, Maaz Khan f, Qasim Khan g, *,
Muhammad Maqbool h, *
a
Physics Department, Lahore Garrison University, Lahore 54000, Punjab, Pakistan
b
Department of Physics, Riphah Institute of Computing and Applied Sciences (RICAS), Riphah International University, 14 Ali Road, Lahore, Pakistan
c
Solar Cell Application Research Lab, Department of Physics, Government College University Lahore, Lahore 54000, Punjab, Pakistan
d
State Key Laboratory of Chemical Resource Engineering, Beijing Advanced Innovation Centre for Soft Matter Science and Engineering, Beijing Engineering Centre for
Hierarchical Catalysts, Beijing University of Chemical Technology, Beijing 100029, China
e
Tianjin Institute of Industrial Biotechnology, Chinese Academy of Sciences, Tianjin 300308, China
f
Nanomaterials Research Group, Physics Division, PINSTECH, Islamabad, Pakistan
g
Institute of Microscale Optoelectronics, Shenzhen University, Shenzhen, Guangdong 518000, China
h
Department of Clinical & Diagnostic Sciences, Health Physics Program, the University of Alabama at Birmingham, USA
A R T I C L E I N F O A B S T R A C T
Keywords: Nanotechnology is one of the emerging fields of the 21st Century. Many new devices and patentable technology
Nanotechnology is based on nanomaterials (NMs). One of the dominant factors in the use of nanomaterials and their applications
Nanomaterials in various fields is the synthesis and growth mechanism of nanostructures and nanomaterials. A nanostructured
Synthesis
material may have been a good candidate in one application but could be more useful in a different application if
Top-down
Bottom-up
synthesized by a different mechanism and technique. Similarly, the structure and morphology of a nanomaterial
also depend upon the method of growth and synthesis. For example, it is easy to grow and synthesize amorphous
nanostructured thin film using the plasma magnetron sputtering technique, but it may be difficult to obtain a
similar structure using the thermal evaporation process due to the nature of the technique itself. In this study, the
Top-down and Bottom-up methods and techniques of synthesizing nanostructured materials are reviewed,
compared, and analyzed. Both approaches are critically analyzed, and the influencing factors on the synthesis of
different nanomaterials, the advantages, and disadvantages of each technique are reported. This review also
provides a step-by-step analysis of the choice of method for the synthesis of namomaterials for specific
applications.
1. Introduction society, and provide solution of current industrial, electronics, national

security, drug delivery, and environmental problems at Nano level
The word ‘Nano’ is a Greek prefix derived from the word dwarf, [1–3]. NMs in the range of 1 to 100 nm have had an increasing interest in
indicate a billionth. One nanometer (nm) presents one billionth part of a the field of science over the last decade such particles are known as
meter. The field of Nanoscience and Nanotechnology has obtained nanoparticles (NPs). NMs have vast applications in medicine, cosmetics,
special importance in the modern technological world applications not packaging, nanofiber, biosensor, and electronics in the present area of
just because all measurements are performed and taken on a nanometer research and received significant attention on behalf of magnetic, cat
scale. This special attention and importance are given to Nanoscience alytic, mechanical, optical, and electronic properties [4,5]. The chemi
and Nanotechnology because down at the nanometer level, Quantum cal, physical properties of nanoscale materials depend upon their surface
phenomena start, which has already brought revolutionary changes in atoms because an increase in surface-volume ratio decreases grain size
science & technology. Nanotechnology has a great impact on our and also melting point of the surface atom which affects chemical and
* Corresponding authors.
E-mail addresses: [email protected] (M. Ikram), [email protected] (Q. Khan), [email protected] (M. Maqbool).
https://doi.org/10.1016/j.cis.2021.102597
Received in revised form 7 December 2021;
Available online 29 December 2021
0001-8686/© 2021 Elsevier B.V. All rights reserved.
N. Abid et al. Advances in Colloid and Interface Science 300 (2022) 102597
Fig. 1. The top-down approach and the bottom-up approach.
physical properties [6]. NMs size can be controlled by different ways

such as limiting concentration, micelle growth arrangement, and func
tionalizing surface of the particle. NMs consisting of three different Fig. 2. Flow chart of classifications of NMs.
layers. The surface layer of NMs will normally consist of metal ions,
polymers, and small molecules. Mostly small molecules are used because • One dimensional (1D): Two dimensions are in the vicinity of
it forms a covalent bond with surface particles and contains groups nanoscale, but the last one is not. This classification includes nano
which can carry a charge. While term shell is the outer layer of inorganic rods (NRs), nanotubes (NTs), NWs.
NMs that have chemically different material from the core. In addition, • Two dimensional (2D): Any one of the dimensions will be in
the core is an essential part of NMs, particular properties of NMs are nanoscale, the remaining two dimensions will be outside of it.
depending upon core composition. The core will play a key role in NMs Nanofilms, nanolayers, NSs are examples.
toxicity but this doesn’t mean that the environmental behavior of NMs • Three-dimensional (3D): Bulk NMs that are larger than nanoscale
will depend on core composition [7]. NMs divided into various types (1–100 nm) dimensions are known as 3D NMs. 0D, 1D, and 2D NMs
included 0D NPs, 1D nanowires (NWs), 2D nanosheets (NSs), and 3D are building blocks in 3D NMs. NCs, core shells, nanowire bundles,
networks [8]. Moreover, origin-based NMs can be divided into three nanotube bundles, multi nanolayers are among them [10]– [12].
main kinds: i) incidental NMs (welding fumes, forest fire, and vehicle
engine exhaust), ii) engineered NMs (chemical manufacturing, airplane 2.2. Carbon-based material
engine, and fuel oil and coal), and iii) naturally produced NMs (animal,
insect and in human bodies) [9]. Top-down and bottom-up are two ways These NMs are made of carbon content and come in a variety of
to approach nanoscale. The top-down approach means reduce the size of morphologies. Fullerenes, Carbon Nanotubes (CNTs), Graphene (GR),
the structure toward the nanoscale. While the bottom-up approach is the carbon nanofibers, and carbon black are some of the different types of
formation of large nanostructure from smaller atoms and molecule [7] carbon NMs [13], shown in Fig. 4.
as depicted in Fig. 1. Main aim of this review paper to discuss properties,
classification and explain detail synthesis of NMs by various top down 2.2.1. Fullerenes
and bottom-up process. Fullerenes (C60) are carbon atoms bound together by sp2 hybridi
zation in a spherical shape.
2. Classifications of nanomaterials It is made out of nanomaterial in the shape of a hollow cage. It at
tracts economic interest because of its electrical conductivity, strength,
On basis of morphology, size, and form, NMs are divided into various structure, electron affinity, and versatility. Pentagonal and hexagonal
categories. Fig. 2 shows classifications of NMs. carbon units make up fullerenes. It could be a single layer or
Some of the most important classes are discussed here. multilayered.
2.1. Dimension-based classification 2.2.2. Carbon nanotubes (CNTs)

CNTs, previously known as buckytubes, are elongated cylindrical
Dimensionality is a key property that can be used to separate distinct fullerenes having.
NMs structures. At least one dimension in the 1–100 nm range is present diameters of nm and lengths in micrometer or millimeters. These are
in NMs [10]. Dimension based NMs, shown in Fig. 3, are classified as. GR-based nano foil made of carbon. They are hollow cylinders with
honeycomb lattice-organized carbon atoms. Based on folding CNTs
• Zero dimensional (0D): All three dimensions of NMs lie in the categorize as single-walled NTs (SWNTs) and multi-walled NTs
nanoscale range. This category includes NPs, quantum dots, nano (MWNTs). These are more durable than steel and can enhance structural
spheres, nanoclusters. integrity.
2
Fig. 3. Schematic diagram of dimension-based NMs.
Fig. 4. Carbon-based NMs reproduced from [13].
2.2.3. Graphene (GR) ingredients for metal nanostructures. Metal ions are converted to metal
GR is an allotrope of carbon, in 2D planar surface, it is a carbon-based NPs using reducing agents. These have a large surface area and a good
hexagonal. ability to adsorb small molecules. Commonly employed in a variety of
honeycomb structure. A 2D sheet is about 1–2 nm thick. scientific, environmental, and other fields [11–13].
2.2.4. Carbon nanofiber

GR nano foil is transferred into carbon nanofiber as CNTs, however 2.4. Semiconductor NMs
instead of cylindrical tubes, nano foil are twisted into a cone or cup.
Semiconductor nanostructures possess both metallic and non-
2.2.5. Carbon black metallic characteristics. By altering it, they show diverse properties
A carbon-based amorphous material with diameters ranging from 20 with broadband gaps. Common in photocatalysis and electronic gadgets
to 70 nm with a. [11].
usually spherical form. There is a lot of interaction between particles,
therefore they are stuck together in a clump [11–15]. 2.5. Nanocomposites
2.3. Metal-based NMs A nanocomposite is a polyphase solid substance with one, two, or all
dimensions less than 100 nm. Considered as materials of the 21st cen
Metal-based NMs are synthesized from metals to nm sizes using tury due to their high performance with unique design possibilities and
destructive or constructive. exceptional property combinations. In contrast to traditional compos
processes. Divalent and trivalent metal ions are the beginning ites, NCs have a high surface-to-volume ratio [11,15].
3
3. Properties of nanomaterial 4.1. Top-down approach
3.1. Chemical properties Transformation of bulk material into small nano-sized particles is
done using this approach. Although top-down approaches are simple to
NMs composition and Chemical structure have an important role to use, they are ineffective for manufacturing irregularly shaped and
provide the desired function. Chemical properties such as surface en extremely small particles. The difficulty in obtaining proper particle size
ergy, chemical potential, oxidation process, and catalysis have a great and shape is the main downside of this approach.
impact on the composition of NMs.
4.2. Bottom-up approach
3.2. Physical properties

The constructive technique is a term used to describe the bottom-up
approach. The bottom-up method is the polar opposite of top-down.
The physical properties of NMs depend upon the size, shape, color,
NMs with well-defined shape, size, and chemical composition are
and morphology of particles. Size effect, crystalline structure, lattice
formed through the growth and self-assembly of atoms and molecules as
parameter, and morphology of NMs are combined effects of size, shape,
their building blocks [10,11,13,14,23]. Fig. 5 depicts some top-down
and arrangement of particles.
and bottom-up approaches.
4.2.1. Mechanical milling or ball milling process of top-down techniques

3.3. Optical properties The simplest and efficient mechanical process of the top-down
approach is ball milling, which produces NPs by attrition. It is the pro
Optical properties of NMs like reflection, light emission, absorption, cess of transferring kinetic energy from the grinding medium to the
and transmission depend on their electronic structure since electronic material being reduced. A variety of NPs and metal alloys are created
structure depends upon surface atoms. Optical properties are used to using this process. Temperature and pressure created by the interaction
observed the size effect when particle size reduction to ~10 nm. between balls, as well as impact between balls and vessel wall, can cause
severe phase transformation at high temperature, a predetermined
amount of powder material is poured in milling vial and treated by
3.4. Mechanical properties friction and interaction between vial and balls. It is employed in various
materials to reduce particle size. Ball milling powder samples have a
The mechanical behavior of NMs leads toward high strength condi prominent impact on, crystallite size, reduction of particles as well as
tions and high-speed plasticity. Mechanical properties of NMs signifi mechanical dislocation, surface modification, and possible development
cantly deal with the influence of grain size, material structure, hardness, of metastable phases. It is possible to produce a variety of reactions that
the influence of porosity, elastic modulus, adhesion, and friction do not occur at ambient temperature [24–29].
[16–22]. The milling process is used for many purposes given below [30].
4. Synthesis of NMs with various approaches and methods • Compression in particle size.
• Growth of particle size.
Methods for synthesizing NMs are classified as top-down and • Change in particle structure.
bottom-up approaches. • Agglomeration.
Fig. 5. Top-down and bottom-up synthesis techniques for nanostructures.
4
Fig. 6. Schematic diagram of ball milling technique.
• Alloying mechanically (solid-state alloying). ▪ Attrition milling

• Mixed phases (two or more materials) are blended. ▪ Mill of attrition is generally a stirred ball mill or attrite. Rota
• Changing or modifying a material characteristic (density, flow- tion of the central shaft, on which secondary arms are fixed,
ability, or work hardening). causes balls to spin. The cylinder is fixed in place.
▪ Horizontal milling
The schematic view of the diagram is shown in Fig. 6. ▪ The horizontal axis of the cylinder revolves. Balls rise and fall
The temperature rises during milling attributable to ball-to-powder, onto powder particles due to a combination of centrifugal force
ball-to-wall collisions, ball-to-ball collisions, and frictional forces. There generated by this rotation and gravity.
are several reasons for the total temperature rise of particles during ▪ Vibratory milling
milling. ▪ Shaker mill is another name for it. The vessel is programmed to
oscillate vertically. The ball rises then falls back upon powder.
• The temperature of powder is raised by severe mechanical defor ▪ Rotatory milling
mation caused by the kinetic energy of the grinding medium (balls). A 3D vibratory mill is a machine that rotates. A Three-axis
As the energy level rises, so does the temperature. shaker is another name for it, operates on the same idea as a
• Exothermic reactions probably occur throughout the manufacturing 1D vibratory mill, but with rotation, it is a little more compli
process. Powder particles burn during the milling process, gener cated. Balls clash with the container’s side walls (friction and
ating extra heat [31]. collisions), as well as its base and top [29,32–48].
Synthesis of several NMs using the ball milling method is demon

4.2.1.1. Influencing factors. The outcome is highly influenced by ball strated. in Table 1.
size, vial volume, the overall mass of balls, rotating speed of the mill,
and amount of powder, milling environment, and milling duration. The 4.2.1.2. Advantages. The milling process has several advantages and
milling process is more impactful when the ball to powder weight ratio is benefits. Some of them are listed below [30,48,49].
higher. As the number of collisions per unit time rises the number of
balls increases, and a smaller amount of powder in the vial, faster is the • High capacity and universality.
velocity of a single ball in the cylinder, greater is the efficiency. • Long-term maintenance of a specified milling fineness by a certain
Planetary mill, attrition mill, horizontal mill, vibratory mill, and capacity (with a periodic supply of balls to compensate for wear).
rotatory mill are some examples, based on the movement of milling balls • Simplicity in serving, reliability, and safety.
and vials. These types are discussed below. • May be used to reduce the thickness of stacked materials.
▪ Planetary milling 4.2.1.3. Disadvantages. Some of the disadvantages of the milling pro
▪ Smaller than a conventional ball mill and is commonly used in cess are also provided here [30,50].
laboratories for research. Comprised of two or more jars that
rotate around their axes including supporting plate’s symmetry • The majority of ball milling treatments are destructive, destroying or
line moves in the opposite direction of grinding jar. Super disordering crystal structure and introducing a large number of
imposed rotational movements are applied to grinding balls. flaws.
Milling medium (balls) inside vials move due to Coriolis effect, • Inconvenience and hefty weight.
combined field of centrifugal forces, shear and compressive • Grinding uses a lot of energy because of wear on balls and wall
forces to powder charge. Just a little amount of powder is armor, friction, and material heating, among other things.
required, the most commonly utilized technique for mechanical • During work, there is a lot of contamination and noise.
alloying.
5
Table 1
Synthesis of NMs by ball milling technique.
Nanomaterials Milling model Milling medium Ball size Powder to ball rpm Time Particle Ref.
ratio size
Graphite oxide (GO) NPs Planetary model Stainless steel and 5 mm – 600 rpm 6 h, 16 h, 24 h, with 10 min – [51]
(2018) zirconia balls break
Bornite Cu5FeS4 NPs High energy Steel balls 6–10 – 1000 5,10,30,60,120 min 10–40 nm [52]
(2018) model mm rpm
ZnO NPs High energy – – 1:100 10–30 nm [53]
(2021) model
ϒ-MgH2 Stainless steel balls 10 mm 1:12 750 rpm 10 h,50 h,72 h [54]
(2019)
CuO- Biochar Planetary – – 1:50 400 rpm 9h 13.8 nm [55]
NCs (2020) model
GR Oxide (GO) NPs Planetary model Stainless steel jar – 1:20 300 rpm 12 h 40 nm [56]
(2020)
magnetite-maghemite Planetary model Steel 3 mm – 200 rpm 24 h, 100 h 10–15 nm [57]
NPs (2018)
Fig. 7. Schematic diagram of thermal evaporation.
4.2.2. Thermal evaporation of a typical thermal evaporation setup is shown in Fig. 7.

It’s an endothermic process in which heat causes chemical break An alumina crucible holding powder was positioned in the center of
down. This heat breaks a chemical link in a molecule [14]. Thermal the heating zone in a typical procedure, with untreated substrate facing
evaporation is one of the most popular methods for producing stable powder [59]. A resistive heating method was used to heat the source and
monodisperse suspensions with self-assembly ability among numerous substrate. A consistent gap of 20 cm is maintained between the source
approaches for the production of inorganic NPs [58]. Thin films are and substrates [60]. Before being placed in the evaporator, substrates
made on a variety of substrates using thermal evaporation. The scheme are cleaned with acetone and ethanol [61]. Using a PID (proportional
Table 2
Synthesis of NMs by thermal evaporation technique.
Nanomaterials Substrate Target Synthesis conditions Particle size Ref.
Tin sulfide (SnS) thin ZnO: Al, glass/ITO, Tin sulfide substrate temperature 400 ◦ C, evaporation time 40 min, chamber Film thickness ~ 720 nm [60]
films and glass/CdS pressure 9 × 10–6 Torr, source and substrate distance 20-cm
(2017)
Zn2GeO4 nano- Au coated Si Zn and Ge Temperature 950 ◦ C, evaporation time 30 min, the distance between thickness 10 nm [63]
crystals powders source and substrate ~10 cm.
(2019)
Ga2O3 thin film quartz Ga2O3 powder source and substrates distance 20 cm, heating current 200 A with a Film thickness 350 nm [61]
(2018) vapor pressure of 3 10–4 Pa.
Cu2InO4 thin film Si Copper and Oxygen flow at 60 standard cubic centimeters (sccm) in a tube furnace _ [64]
(2019) Indium with a pressure of 0.2 × 10− 2 Torr.
MoS2 nanostructures Si pure MoO3 and S A gap of 18 cm was established between two alumina boats. Furnace The thickness of MoS2 [59]
(2018) powders heated to 625 ◦ C at a rate of 15 ◦ C/min for 10 min. flakes is 0.7 nm.
6
integral derivative) controller and a digital display, temperatures at the

source and on a substrate are measured and controlled. Crucible’s
entrance is fitted with a shutter that allows deposition time to be
controlled. Glass slides were cleaned in soap solution before being ul
trasonically washed in acetone and de-ionized water before deposition
[60]. As source materials, stoichiometric powders of each chemical
(99.99%) were utilized individually in crucibles [62]. Thermal evapo
ration has been used to make a variety of NPs, as shown in Table 2.
4.2.2.1. Influencing factors. The process of of thermal evaporation is

influenced by several factors [65–67]. The temperature in the furnace,
evaporation duration, and source to substrate distance are experimental
parameters for the formation of nanocrystals [63]. Using a rotating
pump, the tube furnace was emptied. The tube was filled with oxygen
[64].
4.2.2.2. Advantages. The thermal evaporation process has several

advntages over other processing of synthesis and fabrication. A list of the
advantages is given below [65–67].
• This fabrication procedure does not require any solvents.

• Materials can be deposited on substrates evenly and uniformly, Fig. 8. Schematic diagram of laser ablation technique.
which is especially important for ultrathin layers.
• Monitoring deposition rates of each precursor allows for exact con wavelengths. An excimer laser is a type of pulsed gas laser, produces
trol of film thickness. ultraviolet light having a power efficiency of 0.2 to 2% [68]. As a result,
• particularly suitable for materials with low melting points. the laser has evolved into a potent instrument that may be used to
• Shutters and masks can be used because of line-of-sight trajectory replace traditional micro-processing techniques. Laser processing speed,
and limited-area sources. on other hand, is still too slow for industrial application [71]. Fig. 8
• Monitoring and controlling deposited material is quite simple. shows a schematic diagram of a typical LA setup.
• During deposition, the deposition system can be pumped at a rapid Laser is used in most procedures. A common technique involves
pace. focusing a laser beam on a metal target submerged in liquid, which
• In a vacuum environment, residual gases and vapors can be easily produces vapor, molten metal droplets, or plasma, which subsequently
monitored. react with a liquid medium to create specific compounds and develop as
• Probably the most cost-effective PVD process. NPs [72]. NPs are produced by irradiating a solid target (typically metal)
submerged in a liquid (acetone, ethanol, water, chloroform, iso
4.2.2.3. Disadvantages. Disadvantages of the thermal evaporation pro propanol, etc.) with a pulsed laser beam to generate NPs whose
cess are also provided below [65]. morphology, composition, and other properties may be adjusted by
altering laser settings and liquid medium [73]. Table 3 shows many
• Many alloy compositions and combinations are merely difficult to types of NPs that have been created using laser ablation.
deposit.
• For film property control, there are just a few processing variables 4.2.3.1. Influencing factors. Laser characteristics such as fluency,
accessible. wavelength, repetition rate, and pulse duration, transmission, the light
• Source material may be poor. absorption efficiency of target material, and chemical composition of
liquid all influence ablation rate. As a result, NPs characteristics are
4.2.3. Laser ablation influenced by laser settings as well as liquid media [74].
The term laser refers to a high-intensity beam of electromagnetic
radiation that is amplified through stimulated emission of radiation. 4.2.3.2. Advantages. There are various advantages to laser ablation
Einstein was the first person to propose a laser hypothesis [68]. Syn [75].
thesis of NPs from diverse solvents using laser ablation synthesis in so
lution is a straightforward process [14]. Since Maiman built the first • The ability to generate ligand-free noble NPs in a range of solvents is
practical laser in 1960, lasers have been widely employed in fields of one of the major benefits of LA synthesis in solution.
information transmission, medical treatment, industry, and military • Low loss of energy.
[69]. Laser ablation (LA), which utilizes a pulsed laser to remove mol
ecules from a substrate surface to create micro/nano structures, has
4.2.3.3. Disadvantages. Laser ablation also possess afew disadvantages
numerous applications in metals, ceramics, glasses, and polymers. LA is
given below [74].
a top-down method of eliminating the substance from a substrate by
focusing a laser beam above it. Only when a substance absorbs enough
• To get a high ablation efficiency, a lot of energy is required.
energy to melt or evaporate does ablation occur. In laser machining
• On an industrial scale, even the most dispersed laser sources are
applications including high-precision drilling, laser beam milling, and
incapable of creating NPs.
laser cutting, the overall process of laser ablation is constant. Ablation is
• Due to the large number of NPs distributed along laser beam, abla
a term that refers to a process that involves both vaporization and melts
tion effectiveness drops with increased ablation duration.
ejection [68]. Following are the most frequent near-infrared laser
sources: Nd: YAG lasers generating at 1064 nm and 800–970 nm is a
4.2.4. Sputtering
range for Diode lasers emitting [70]. Infrared lasers and UV/excimer
Sputtering is more prominent among bottom-up approaches due to
lasers are two types of laser sources that may be classed by their
its non-thermal vaporization process. The sputtering process can be
7
Table 3
Synthesis of NMs by laser ablation technique.
Nanomaterials Laser light source Ablation duration Pulse width Wavelength Frequency Target Particle size Fluence Ref.
(min) (nm) (Hz) material (nm) (J/cm2)
Carbon based Nd: YAG Laser 10 6 ns 532 10 Graphite 200 0.4 [76]
NMs
TiO2 and ZnO Nd: YAG laser 30 2.0 ms 1064 5 Zn and Ti 5–65 – [72]
plates
TiO2 Nd: YAG 5 10 ns 1064 and 532 10 titanium rod 1 to 40 45.9 and [77]
27.6
ZnO Nd: YAG 30 7 ns 1064 10 zinc 18 12.7 [69]
Carbon based NPs Nd: YAG 5 ms 1064 2 Graphite 80 to 130 [78]
_ _
SnO Nd: YAG 15 0.5 ms or 2.0 1064 3 Sn/Zn 30–60 [73]
and ZnO NPs. ms _
CdO NPs Nd: YAG 10 7 ns 1064 10 Cd sheet 24 _ [79]
Ag NPs Femtosecond 15 40 fs 1000 silver 13 to 18 _ [80]
laser _
ZnO NPs Nd: YAG 3 7 ns 1064 20 Zn target 18–26 _ [81]
Iron Oxide MNPs Nd: YAG 5 7 ns 1064 20 Fe target 2–80 150 [82]
Fig. 9. Schematic diagram of sputtering technique.
attained at <0.67 Pa, low pressure will maintain by using a vacuum ions attack a nonconducting target which leads to charge a surface. Ion
pump [83]. Different components of the sputtering system include: 1) current would die off. Therefore, dc-sputtering is restricted to con
evacuated chamber 2), sputtering source 3), gas supply 4), electrode 5), ducting materials like metals or doped semiconductors [87]. Oxygen
substrate holder [84]. A systematic diagram of the procedure is shown in and nitrogen are used as reactive gases, when one of them is added into
Fig. 9. the sputtering chamber, this gas will provide a reaction with the target
In the process of sputtering, NMs are deposited on a substrate’s surface and sputtered atom, thus form a chemical compound thin film on
surface by ejecting particles with the attack of high-energy ions. The the substrate. This type of sputtering is named reactive sputtering [88].
sputtering process is used for surface coating, thin layer deposition, and Furthermore, plasma ions behave as a neutralized electric charged
surface etching application [13,85]. Glow discharge sources are working when they strike with the target and then return to process as an atom. If
by applying an electric potential between the electrode in a gas phase in the insulator is used as target material, then due to the process of
a low-pressure environment. As electrons accelerated and collide with a neutralization positive charges are appeared on the target spot. This
gas atom, such ionized gas is called plasma. These plasma ions are the positive charge may reach a level at which energetic ions are repelled
simplest source for sputtering [86]. and it will end the sputtering process. In this situation by reversing the
In the direct current (DC) sputtering process, a negative voltage is polarity process can continue and attract a maximum electron from
applied in presence of Ar-ions toward the target and set material free, in plasma to eliminate the surface charge. Periodic reversal of polarity is
this result secondary electrons are produced. Further ionization of gas is done automatically by applying a radio-frequency (RF) voltage on the
caused due to these secondary electrons. Under an electric field, positive target. Thus, this type of sputtering is called RF sputtering [89]. The
8
efficiency of the Sputtering technique will be increased by using • Expensive equipment.

magnetron sputtering. In the magnetron sputtering technique, the
magnetic field is used to a deposited thin film on the substrate. Plasma 4.3. Bottom-up approaches
should enhance by trapping electrons in a magnetic field around the
target by using a magnetic field. This result increases the ionization of 4.3.1. Chemical vapor deposition
argon atoms and bombardment ions that increase deposition rate [90]. CVD is a diverse and successful method for creating nanostructures.
This technique has a lot of benefits as compared to other sputtering In the industry of microelectronics, CVD was a major technique for de
processes such as high deposition rate, homogeneity, control of thick cades and is still one of the most appealing methods today capable of
ness, great adhesion deposition over a comparatively large area, and addressing obstacles that modern technologies imply [107]. NMs are
also used with RF and DC sputtering. RF and DC magnetron sputtering is created with this process using relatively simple materials. A thin
differentiated on basis of AC and DC source mood respectively [91,92]. coating of gaseous reactants is placed on a substrate using this approach.
Schematic diagrams of DC and RF are shown in Fig. 10. In a reaction chamber, when gas comes into touch with a heated sub
Ion beam sputtering is a different method as compared to others. In strate, a chemical reaction happens [108]. As a result, a thin layer is
it, ion beam from source ion direct sputter on target and plasma from formed on the substrate surface. This thin film is etched out and put to
which ions are released are isolated inside discharge vessel of the ion good use.
source. It means there is no contact between working gas and substrate Operating requirements are as follows: controlled delivery of gas-
[93]. Sputtering deposition efficiency can be improved by increasing phase reactants, availability of an enclosed reaction chamber,
deposition rate, decrease the dark area in the deposition chamber, discharge of gases, regulation of reaction pressure, delivery of energy
increasing plasma ionization, and increasing bombardment ion effi source for chemical reactions, cleanup of exhaust gases to achieve safe
ciency [94]. Synthesis of several NMs using the sputtering method and nontoxic levels, and automation process control to increase depo
illustrated in Table 4. sition process’s stability [109].
4.2.4.1. Influencing factor. Factors affecting the sputtering process are 4.3.1.1. Mechanism. Reactant gases are first delivered toward the
given below [13,91,95,96]. reactor. These reactant gases just either proceed through homogeneous
reactions in the gas phase to create intermediate reactants and by-
• Annealing duration, Temperature, and thickness of layer are products of gases, or they diffuse directly on the substrate via bound
different parameter which determines size and shapes of NPs. ary layer in both conditions, intermediate reactants and reactant gases
• The angle of target and substrate. adsorb and diffuse onto the heated substrate surface. Evaporation of
• Mass and energy of bombarding particle. growing species for transport to a substrate where they assemble and
• Ar+ ions presence in vacuum system. grow through a carrier gas. Consequent heterogeneous reactions at the
• Substrate temperature to reduce dopant redistribution. gas-solid interface lead to continued thin-film production, as well as
generation of reaction by-products, via coalescence, growth, and
4.2.4.2. Advantages. The sputtering process has several advantages nucleation. Eventually, unwanted gaseous products and undissolved
over others. Some of them are listed below [97,98]. species desorb from the reaction zone’s surface and are removed.
Whenever the temperature is sufficiently enough or more energy is
• Sputtering techniques can work at low temperatures. supplied, such as in form of plasma, gas-phase processes occur.
• It can coat large areas more uniformly. Furthermore, if deposition reaction is dependent on substrate surface
• The sputtering deposition target provides a stable, long-lived catalysis, as with specific metal surface catalytic growth, a heteroge
vaporization source. neous reaction is required [110–113]. Fig. 11 shows a schematic dia
• Elements, alloys, and compounds can all be sputtered and deposited. gram of the procedure.
4.2.4.3. Disadvantages. Some of the shortcomings and disadvantages of • Cooling system to room temperature.
the sputtering process are listed here [98,99]. • Introducing a constant flow of carrier gas at a particular pressure.
• Heat up substrates to suitable substrate temperature.
• Sputtering rates are low compared to thermal evaporation. • Heating source to suitable temperature (beginning of growth).
• Most of the energy is converted into heat when incident on target, • Chilling source to heating rate (ending of growth).
which must be removed. • Cooling at room temperature.
• Low purity.
Fig. 10. DC and RF mode of sputtering.
9
Table 4
Synthesis of NMs by using sputtering technique.
Nanomaterials Target material/ Substrate Sputtering Method Sputtering gas Pressure/Temperature/Duration Particle Size Ref.
− 7
CuO Copper/ Copper Reactive magnetron Ar/O2 = 40/10 7.4 × 10 Torr/24 h ~9 nm [100]
(2016) cold finger
− 2
Cu Copper/ Silicon DC Sputtering Ar 20sccm 2 × 10 Torr/7,15 and 30 s 37.8 nm 25.4 nm 19.6 nm [101]
(2017) Oxide
Pt Pt/ Polyethylene glycol Matrix Ar 30 ◦ C/30 min 0.9 ± 0.3 to 1.4 ± 0.3 nm [102]
(2018) Sputtering
Pd Pd/ Mesoporous silica Sputtering deposition Ar 2 × 10− 7 mbar/ 9 nm at 7.5 min, 15 nm at 12 min [103]
(2018) 0.5–12 min
Fe3O4 Fe/ Si DC Sputtering Ar and O2 4 × 10− 3 mbar 50 nm and [104]
(2017) 150 nm thick film
− 4
Fe Fe/ Si-SiO2 Gas flow sputtering Ar 490sccm 4 × 10 Pa 20–25 nm [105]
(2020)
8
ZrO2 Zirconium/ Copper cold finger Reactive magnetron Ar/O2 = 40/10 7.6 × 10− Torr/60 h 2 nm to 8 nm [106]
(2018)
Fig. 11. Schematic diagram of CVD technique.
Table 5
Synthesis of NMs by CVD technique.
Nanomaterials Catalyst Substrate Precursor Temperature Time Target Particle size Ref.
(min)
GR film – Copper Ethanol 850 ◦ C 5–6 GR – [117]

(2020) min
MoxW1-xTe2 – SiO2/Si Mo (w) & Te 710 C ◦
30 – 50 nm [118]
nanobelts (2018) min
GR nanoplatelets nickel – waste cooking oil 850 ◦ C, 875 ◦ C, and 5 min – [119]
(2018) oxide 900 ◦ C,
N- doped CNTs Fe2O3 Silicon Acetylene – 2 min – – [120]
(2017)
ZnO film – Alumina ceramic and Zinc acetate dehydrate, 400C – – ZnO-c ~ 220 nm and [121]
(2020) glass ZnO-p ~ 350 nm
CNTs – Ferrocene aerosol Acetylene 1000C – – – [122]
(2018)
F-doped SnO2 thin – Pilkington silica- Sol. Of ammonium fluoride 550 ◦ C 5 min – 150–500 nm [123]
films coated barrier glass monobutyltin trichloride
(2017) BuSnCl3 and methanol
• When heating and cooling, use a high carrier gas pressure and only in Table 5.
introduce the required procedure pressure while the source is at the
right temperature. 4.3.2. Influencing factors
The formation of NMs may be adjusted by adjusting CVD parameters.
The synthesis of several NMs using the CVD method is demonstrated At moderate pressure, processes take place, similarly operate at mild
10
pressure (1 Torr) or ultrahigh vacuum (100 Torr). In regards to coating temperature difference should be kept between the upper and lower
uniformity, pressure has a significant impact on the quality of products portion of the chamber. After it, ions are transferred toward the low-
and deposition rate. Gas flow state, substrate and physical characteris temperature region, and seed crystals are deposited at the cooler end,
tics of vapor, deposition time, precursor nature, catalysts, temperature to collect the desired crystal.
[500]. Most conventional CVD technique is carried out at extreme Step 3: After centrifuge, washed and then dried sample at different
temperatures, usually about 1000 ◦ C; however, CVD at a moderate temperatures to acquire final product.
temperature (about 300 ◦ C) is used while substrate can’t sustain high Crystal morphology under hydrothermal conditions is closely related
temperatures [110,114]. to growth conditions. The mechanism of crystal growth was predicted by
morphology study. To control the morphology of prepared material,
4.3.3. Advantages either low pressure or high-pressure state can be used depending mainly
The CVD method has several advantages over other methods of on the vapor pressure of the main reaction composition. Hydrothermal
nanostructures growth and fabrication. A list of those advantages is synthesis is used for important solids preparations such as luminescence
given below [107,115,116]. phosphors, superionic conductors, and microporous crystals. It is also a
route to unique condensed material, including thin films, nm particles,
• It has the finest degree of control. and gels [23,89,124–129]. The hydrothermal mechanism is shown in
• Allows for large-scale fabrication of 2D NMswith purity, good crystal Fig. 12.
quality, and few substrate flaws.
• Material production is dense and pure. 4.3.6. Influencing factor
• Controlling process parameters allows regulating crystal structure, Various factors can affect the synthesis and fabrication of nano
surface morphology, and orientations of nanostructures. structured material using hydrothermal technique [130]. Those factors
• The synthesis procedure is repeatable. are listed below.
• Material adherence and homogeneity on the substrate are excellent
enables for complicated shaped coatings. • High temperature and pressure.
• Produces extremely hard, robust, homogeneous, and pure • Reaction time.
nanostructures. • Solvent type.
• The growth rate can be easily regulated.
• The classical CVD approach has a reasonable processing cost. 4.3.7. Advantages
Several advantages, the hydrothermal technique may have over
4.3.4. Disadvantages othrr parallel techniques, are listed below [23,131].
The CVD method has several advantages over other methods used for
the same applications. However, there are some disadvantages also • Precise control of size NPs.
associated with the CVD method. Those disadvantages are listed below • Low melting point, high vapor pressure, and tendency toward py
[107,115,116]. rolysis will be obtained.
• Produce nanocrystal with high crystallinity
• Material is transferred from deposited substrates for further evalua
tion. Aside from that, the increased production cost is a 4.3.8. Disadvantages
disadvantage. The hydrothermal method of synthesizing nanomaterials have some
• Few precursors are poisonous, flammable, or explosive and few are limitations as compared to other methods. Those limitations are pro
quite costly. vided below [23,125,131].
• Several CVD varieties raise fabrication costs.
• Due to the high deposition temperature of various CVD variations, • Crystal growth information cannot observe directly
there are limitations on used substrates. • Expensive autoclave
• Creates of very poisonous gaseous byproducts.
4.3.5. Hydrothermal method

Hydrothermal synthesis is defined by the reaction of solid material
with an aqueous solution in a reaction vessel at high temperature and
pressure and leads toward small particles deposition. Hydrothermal is a
solution reaction-based approach. The process is referred to as hydro
thermal because water is used as a solvent in this method. The hydro
thermal process is performed in a steel pressure vessel also define as an
autoclave where processing conditions are controlled by adjusting
temperatures and/or pressures. Temperature is increased beyond the
boiling temperature of the water, attaining vapor saturation.
The hydrothermal method has a great contribution to modern sci
ence and technology due to homogenous precipitation, low cost,
friendly environment, easy scaling up, and pure final product. Moreover,
the hydrothermal method can be divided into hydrothermal synthesis,
treatment, and crystal growth, treatment of organic wastes, and prepare
functional ceramic powder. Crystal growth performed by the hydro
thermal method have following step such as:
Step 1: In the concern solution precursor is mixed in a solvent, metal
hydroxide is used as mineralizer and metal alkoxides serve as a source of
metal ions.
Step 2: Hydrothermal treatment is done in a sealed reactor, known as
autoclave, in which nutrient is supplied along with water and Fig. 12. Schematic diagram of hydrothermal technique.
11
Table 6
Syntheses of NMs by using the hydrothermal technique.
Nanomaterials Reducing & Stabilizing Agent Precursor Hydrothermal Synthesis Condition Particle Ref.
Autoclave Size
Ag NPs Nanocellulose AgNO3 Filled 50 mL Teflon- Centrifuged, 86 nm [132]

(2018) 20 mL 0.1 mL ~ 0.5 mL lined washed & dried
Au NPs Hydrolyzed spider cobweb 33 HAuCl4 Filled 50 mL Centrifuged, washed with ethanol for 5 40 nm [133]
(2020) mL 330 mg Teflon vessel min & dried
CuO NPs NaOH 10 mmol & 1 mL Cu (NO3)2.3H2O 10 Filled 60 mL Washed with ethanol & dried ~27.7 nm [134]
(2018) ethylene Diamine mmol Teflon-lined
Fe3O4 NPs 50 mg polyvinyl FeCl3.6H2O Filled 75 mL Filtered, washed & dried 3 h at300◦ C ~65 nm [135]
(2014) pyrrolidone & 25 mL NH4OH Teflon-lined
NiO NPs 50 mM urea Ni (NO3)2 Filled Centrifuge, washed & dried 5 h at 50 C annealed 5 h
◦
20–50 nm [136]
(2020) ⋅6H2O Teflon-lined at 450 ◦ C
ZrO2 NPs NH4OH ZrOCl2⋅8H2O Filled Centrifuge, washed with acetone & dried at 90 ◦ C,
(2018) 0.85 g Teflon-lined calcined at 450 ◦ C for 60 min 12 nm [137]
TiO2 NPs 0.5 g BMI. Cl 0.4 g TiO2 Filled Teflon tube Centrifuge, washed with ethanol & dried in oven at 35 nm [138]
(2017) 80 ◦ C, overnight
• Difficult to Control employed precipitants in this approach. Precipitates are then aged to
produce bigger particles, which are then collected via filtration or
Parameters and synthesis conditions of several NMs using the hy centrifugation. To remove contaminants and obtain high purity NPs,
drothermal method are demonstrated in Table 6. additional wash with ethanol, distilled water, or other solvents are
required. To obtain NMs with desired crystal structures and morphol
4.3.9. Co-precipitation method ogies, post-treatment such as annealing, sintering, or calcination is used.
One of the earliest wet chemical processes of NMs synthesis is co- Fig. 13 shows a schematic diagram of the procedure.
precipitation. This is the most basic and extensively used approach for It entails the occurrence of nucleation, growth, coarsening, and
producing a wide range of NMs. Impurities precipitate along with the agglomeration simultaneously. Nucleation is a crucial phase in the
product in this process, although, can be easily separated using different precipitation process, it is the process by which the tiniest elementary
methods such as filtration and washing. The coprecipitation approach particles of a new thermodynamic phase appear. A high concentration of
refers to the use of a precipitation reaction to achieve a consistent nuclei results from fast nucleation., yielding nanocrystals of smaller size,
composition of two or more cations in a homogeneous solution. Through whereas, slow nucleation results in lower concentration and bigger
numerous chemical reactions in solution, this approach has the advan particles. To minimize the surface energy of smaller particles during the
tage of directly producing homogenous NMs with small sizes and size growth phase, they will be absorbed by bigger particles. Coarsening, or
distribution. The solution is combined directly or drop-by-drop with Ostwald ripening, is the name of the process. Agglomeration could also
another solution containing dissolved precipitation agents, like sodium occur to reduce surface energy. Particles may continue to expand
hydroxide, ammonia, and many more for retaining up essential pH. beyond nanoscale if coarsening and agglomeration are not controlled.
Hydroxides, chlorides, carbonates, and oxalates are the most widely To stop growth, some capping or stabilizing chemicals are beneficial.
Fig. 13. Schematic diagram of co-precipitation technique.
12
Table 7
Synthesis of NMs by co-precipitation technique.
Nanomaterials Precursors pH balance Surfactant added Synthesis conditions Particle size Ref.
NiFe2O4 NPs FeCl3 + NiCl2 NaOH Oleic Stirred 30 min at 80 C, washed, centrifuged, dried
◦
28 nm [144]
(2017) overnight at 80 ◦ C.
ZnO NPs Zn(ac2).2H2O NaOH – Stirred 2 h at 60 ◦ C, centrifuged at 4500 rpm for 2 140 nm [145]
(2018) min, washed, the powder was obtained by drying 6 h
in the oven at 75 ◦ C.
SnO2 NPs SnCl4.5H2O Aquas – Precipitate filtered, washed, and dried at 80 ◦ C for 24 – [146]
(2018) ammonia h, calcined 1 h in the oven at different temperatures
(500 ◦ C, 700 ◦ C, 900 ◦ C).
Fe2O3 NRs FeCl2 NaOH – Heated 3 h at 85◦ , centrifuged, washed, dried at 60 ◦ C Length, [147]
(2017) FeCl3.6H2O+ overnight, calcined 4 h at 600 ◦ C. 110–120 nm
propanol Width,
25–40 nm
Mn3O4 nanograins MnSO4.H2O NaOH Cetyltrimethylammonium Filtered using Whatman filter paper, washed with 600-800 nm [148]
(2018) bromide (CTAB) water and ethanol, dried at 100 ◦ C for 6 h, calcined 2
h at 800 ◦ C.
Cu-doped hematite FeCl3,6H2O+ NaOH – Heated 3 h at 80 ◦ C, centrifuged, washed, dried 3 h at 21 nm [149]
(α-Fe2O3) NPs CuCl2,2H2O 80 ◦ C, calcined 4 h at 700 ◦ C.
(2017)
CoMn2O4 NPs MnSO4.H2O NaOH Cetyltrimethylammonium Stirred 3 h, precipitate washed with ethanol, dried in – [150]
(2020) bromide (CTAB) a hot air oven at 60 ◦ C for 12 h, kept 2 h in a muffle
furnace at 600 ◦ C.
ZnFe2O4 NPs ZnCl2 + FeCl3 NaOH – Heated at 80 ◦ C for 3 h, centrifuged, annealed 24 h at 8.2 nm [151]
(2017) 75 ◦ C, calcined 5 h at 500 ◦ C.
Fe3O4 NPs FeCl3.6H2O + HCl NH4OH Tetramethylammonium Washed, dried 24 h at room temperature. 31.5 nm [152]
(2019) FeCl2.4H2O + HCl hydroxide (TMAOH)
MnFe2O4 NPs (2018) Mn(nO3)2.4H2O + NaOH Stirred 1 h at 70 ◦ C, cooled, washed, sintered 5 h at 36 nm [153]
Fe (NO3)3 600 ◦ C.
Through chemisorption of charged species, capping agents bound to as stirring speed, vibration, light exposure, and glassware cleanliness
particles surface and cause electrostatic repulsion on its surface. Stable impact on quality of NMs produced.
particles will form if repulsive forces are strong enough, otherwise,
coagulation will ensue. It is used for the synthesis of NTs, NRs, and 4.3.9.2. Advantages. Certain benefits to using the coprecipitation
various NPs. Synthesis of various NMs using co-precipitation method approach [10,11,89,139–143].
illustrated in Table 7.
• Easy and quick to prepare
4.3.9.1. Influencing factors. Control of chemical homogeneity and par • Low-temperature, energy-efficient
ticle size is difficult. Recent improvements, such as the use of surfac • Several options for modifying particle surface state and overall ho
tants, have aided in the proper regulation of morphological traits. mogeneity are available.
Furthermore, proper control of experimental parameters such as pH,
reactant and ion concentrations, and temperature is critical because 4.3.9.3. Disadvantages. There are several drawbacks to consider
these factors influence the precipitation process. Working variables such [10,11,89,139–143].
Fig. 14. schematic diagram of sol-gel technique.
13
• If reactants have significantly differing precipitation rates, this due to the separation of water and organic components to produce a gel
approach will not work that disrupts structure. Different drying methods are available: thermal
• Impurities in the product may also precipitate drying gives xerogel, supercritical drying is done to get aerogels and
• It necessitates the employment of numerous chemicals and may freeze-drying is used to obtain cryogel, each has a unique impact on gel
result in the generation of potentially hazardous waste, furthermore, network structure.
most chemically precipitated NPs require stabilizers, as well as a Step 5: Finally, calcination is carried out to get rid of water mole
variety of post-processing procedures to optimize the purity of final cules and residues from the sample. The temperature of calcination is a
products. critical factor in managing material density and pore size.
The process may produce a variety of materials, including thin films,
4.3.10. Sol-gel method NPs, glass, and ceramics. Synthesis of different NMs by sol-gel technique
The most common bottom-up approach is sol-gel for the synthesis of is shown in Table 8.
NMs due to its simplicity. It is a combination of two terms sol and gel. Sol
is a type of colloidal solution made up of solid particles suspended in a 4.3.10.1. Influencing factors. Factors including PH, speed and duration
liquid. The gel is a solid macromolecule that dissolves in a liquid. of stirring, and temperature and time for reaction, greatly affect
The method involves steps: hydrolysis, polycondensation, aging, microstructure, porosity, crystallinity, and densification of the final
drying, and calcination, shown in Fig. 14. product. Solvent and precursor characteristics utilized in the sol-gel
Step 1: Precursor such as metal alkoxide (M-OR) undergoes hydro method have a significant impact on the attributes of products.
lysis with water or alcohol, resulting in the formation of hydroxide so Texture and surface qualities of materials can be controlled very well
lution. If the reaction medium is water, it’s termed an aqueous sol-gel with this procedure. To obtain NPs with correct crystal structure, size,
approach and if the reaction medium is an organic solvent, it is a and crystallinity, heat treatment is essential.
nonaqueous sol-gel method. The General chemical reaction of the hy
drolysis process is described by eq. (1). 4.3.10.2. Advantages. The sol-gel method has numerous advantages,
M − OR + H2 O M − OH + R − OH (1) including [10,11,14,89,139,140,154,155].
Here, M = metal, R = alkyl group. • It is cost-effective.

Step 2: This phase involves condensation of neighboring molecules, • The homogenous character of material produced.
resulting in the removal of water and alcohol resulting formation of • Low processing temperature.
metal oxide bonds. Polycondensation raises the viscosity of the solvent, • The approach is a simple technique to make composites and
resulting in the formation of a porous structure retaining a gel-like liquid complicated nanostructures.
phase. The General chemical reaction of the process is demonstrated by • Allows introduction of modest amounts of dopants into sol that is
eq. (2). equally spread in the final product.
M − OR + M − OH→M − O − M + R − OH (2) • The purity of products is higher.
Step 3: In this step, within the localized solution, polycondensation 4.3.10.3. Disadvantages.
continues, and the gel network reprecipitates. As a result, the porosity of
colloidal particles reduces and thickness between them increases. Aging • There are some disadvantages to employing this strategy as well
causes gel structure and characteristics to vary significantly. [10,11,14,89,139,140,154,155].
Step 4: Afterwards, the gel is dried. Drying is a difficult procedure
Table 8
Synthesis of NMs by sol-gel technique.
Nanomaterials Precursors pH Synthesis conditions Drying process / Particle size Ref.
balance Gel formed
Fe doped TiO2 Iron (III) chloride 6-hydrate, C12H28O4Ti, – Stirred at 40 ◦ C, refluxed at 120 ◦ C for 6 h, gel Supercritical / 6–11, 22–30, [156]
NPs ethanol, citrate acid, C5H8O2 obtained by heating 14 h at 80 ◦ C, dried at 150 ◦ C for Aerogel 50–100 nm
(2017) 1, annealed 1 h at 400, 600, 800 ◦ C.
Bismuth ferrite Bi (NO)3.5H2O, ethylene glycol, Fe – Stirred 2 h, heated at 60 ◦ C, calcined 4 h at 500 ◦ C. Evaporation / – [157]
NPs (NO)3.9H2O Xerogel
(2018)
Al doped ZnO Zn (CH3COO)2.2H2O, Al (NO3)3, methanol NaOH Stirred 90 min, stirred 60 min after balancing pH, – 20–50 nm [158]
NPs centrifuged 20 min at 10,000 rpm, washed, dried 2 h
(2017) at 60 ◦ C, calcined 2 h at 200 ◦ C.
Cd2V2O7 NPs Cd (NO3)2.4H2O, NH4VO3, citric acid, – Stirred 2 h at 100 ◦ C, evaporation formed gel, dried – 10–20 nm [159]
(2018) in oven at 80 ◦ C, calcined 2 h at different
temperature.
CuO NPs Cu (NO3)2.3H2O, citric acid – Stirred at 90 ◦ C till gel formed, heated at 100 ◦ C, – [160]
(2018) annealed 2 h at different temperature 200, 300, 400,
500, 600 ◦ C.
ZnO NPs ZnAc2,2H2O NaOH Heated at a temperature ranging 0 to 80 ◦ C, the Freezing / 37 nm [161]
(2017) precipitate was centrifuged, washed, dried by Cryogel
lyophilization.
Co3O4 NPs Cobalt acetate, polyvinylpyrrolidone – Stirred 30 min, heated 2 h at 300 ◦ C, annealed 3 h at – 50 nm [162]
(2019) (PVP), triethanol 450 ◦ C.
Cu doped TiO2 Titanium butoxide (C16H36O4Ti), copper – Stirred 2 h at 50 ◦ C, annealed at 400 ◦ C. – – [163]
NPs acetate (Cu (CH3COO)2), HCl, methanol,
(2020) ethanol
MnFe2O4 NPs Mn (NO3)2.4H2O, Fe (NO3)3, citric acid NaOH Heated up to 70 ◦ C, evaporated to form gel, dried to – 45 nm [153]
(2018) get flakes, calcined under nitrogen atmosphere 2 h at
900 ◦ C.
14
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Synthesis of nanomaterials using various top-down and bottom-up

Article in Advances in Colloid and Interface Science · December 2021

Namra Abid Aqib Muhammad Khan

Sara Shujait Kainat Chaudhary

Multi-functional Electrolysis View project

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Contents lists available at ScienceDirect

Advances in Colloid and Interface Science

Synthesis of nanomaterials using various top-down and bottom-up

1. Introduction society, and provide solution of current industrial, electronics, national

Fig. 1. The top-down approach and the bottom-up approach.

physical properties [6]. NMs size can be controlled by different ways

2.1. Dimension-based classification 2.2.2. Carbon nanotubes (CNTs)

Fig. 3. Schematic diagram of dimension-based NMs.

Fig. 4. Carbon-based NMs reproduced from [13].

2.2.4. Carbon nanofiber

3. Properties of nanomaterial 4.1. Top-down approach

3.2. Physical properties

4.2.1. Mechanical milling or ball milling process of top-down techniques

Fig. 5. Top-down and bottom-up synthesis techniques for nanostructures.

Fig. 6. Schematic diagram of ball milling technique.

• Alloying mechanically (solid-state alloying). ▪ Attrition milling

Synthesis of several NMs using the ball milling method is demon­

Fig. 7. Schematic diagram of thermal evaporation.

4.2.2. Thermal evaporation of a typical thermal evaporation setup is shown in Fig. 7.

integral derivative) controller and a digital display, temperatures at the

4.2.2.1. Influencing factors. The process of of thermal evaporation is

4.2.2.2. Advantages. The thermal evaporation process has several

• This fabrication procedure does not require any solvents.

Fig. 9. Schematic diagram of sputtering technique.

efficiency of the Sputtering technique will be increased by using • Expensive equipment.

Fig. 10. DC and RF mode of sputtering.

Fig. 11. Schematic diagram of CVD technique.

GR film – Copper Ethanol 850 ◦ C 5–6 GR – [117]

4.3.5. Hydrothermal method

Ag NPs Nanocellulose AgNO3 Filled 50 mL Teflon- Centrifuged, 86 nm [132]

Fig. 13. Schematic diagram of co-precipitation technique.

Fig. 14. schematic diagram of sol-gel technique.

Here, M = metal, R = alkyl group. • It is cost-effective.

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Synthesis of several NMs using the ball milling method is demon