Type of contribution:

Editorial Mechanical Engineering

Research Paper
Case Study for Society and Industry
Review Paper Vol. 1, No. 2 (2021) pp 54-77
Scientific Data https://doi.org/10.31603/mesi.5493
Report of Tech. Application

Recent Progress on the Production of Aluminum Oxide

(Al2O3) Nanoparticles: A Review
Adzra Zahra Ziva1, Yuni Kartika Suryana1, Yusrianti Sabrina Kurniadianti1, Risti
Ragadhita1, Asep Bayu Dani Nandiyanto1*, Tedi Kurniawan2
1 Department of Chemistry, Faculty of Mathematics and Natural Sciences Education, Universitas Pendidikan
Indonesia, Bandung 40154, Indonesia
2 Engineering Technology Department, Community College of Qatar, Doha, Qatar
[email protected]

This article Highlights:

contributes to:
• Reviews on the production of
aluminum oxide (Al2O3) was carried out
• Data obtained from research
publications in 2004-2021
• Perspective advantages and
disadvantages of the synthesis process
have been reported
• Precipitation method is one of the
best methods

Abstract
This study aims at discussing several methods to produce aluminum oxide (Al2O3) synthesis
methods along with the advantages and disadvantages of each method used. In general, several
methods are available: (1) precipitation, (2) combustion, (3) sol-gel, (4) wet chemical, (5) synthesis
in supercritical water conditions, (6) microwave, (7) mechanochemical, and (8) hydrolysis, and the
most efficient method for synthesizing Al2O3 is precipitation because it is facile and the simplest
method (compared to other methods), can be proceeded using inexpensive raw materials,
produces less pollution, and has several advantages: high purity product, high thermal stability,
nearly homogeneous nanoparticle in size, and control desired particle size. The results of the study
help to provide comparisons in producing various Al2O3 synthesis methods.

Article info Keywords: Al2O3, Alumina, Aluminum oxide, Synthesis methods, Nanoparticles
Submitted:
2021-07-09
Revised: 1. Introduction
2021-08-22
Accepted: Nanoparticles or materials that are already small can cause physical and chemical properties
2021-08-28 to alter, resulting in new phenomena. Biomedical research, natural science, and science
applications all benefit from nanoparticles. Drug transporters, cancer therapy, and cell imaging can
Online first: all be done with nanoparticles [1,2]. In monolithic refractories, nanoparticles of α-Al2O3 with a
2021-09-08
narrow size demonstrate good flowability and can be used in radiators or sandpaper [3]. Aluminum
oxide also can be used for microelectronic, catalysis, technical ceramics, and refractories [4]-[8].
Multi-phase nanoparticles are systems with diameters ranging from 1 to 100 nanometers.
This work is licensed under These materials have shown chemical, electrical, optical, mechanical, and magnetic properties that
a Creative Commons differ from bulk materials and their individual atomic constituents. Because nanoparticles have a
Attribution-NonCommercial 4.0 larger surface area than micro and macroparticles, they are frequently used as adsorbents and
International License catalysts [9,10].
Publisher Alumina is a chemical compound of aluminum oxide with the formula Al2O3. Alumina can be
Universitas Muhammadiyah synthesized into several phases such as alpha, beta, gamma, and delta, with each phase reached
Magelang at a different temperature during the synthesis process. Each phase has its properties with other
uses. Alumina is often used in various applications because of its unique properties, such as

Mechanical Engineering for Society and Industry, Vol.1 No.2 (2021) 54

 Adzra Zahra Ziva, et al.

chemical and thermal stability, relative strength, good wear resistance, high hardness, high melting
point, and good electrical and chemical resistance. This material can also act as a mediator in some
chemical reactions [11,12].
In this article, we discuss the Al2O3 synthesis method. This article contains the methods and
the advantages and disadvantages of Al2O3 synthesis. In this study, we found several ways to
synthesize Al2O3 such as precipitation [13]-[26]; combustion [1], [27]-[30]; sol-gel [11,12], [30]-[37];
wet chemical [38]-[41]; synthesis water under supercritical water conditions [33]; microwave [44];
mechanochemical [41,44]; and hydrolysis [45]. Therefore, this paper aims to provide a review of
what methods can be used and which method is more efficient in the Al 2O3 synthesis process. It is
hoped that this paper can positively affect the Al2O3 manufacturing industry in terms of production
costs (economic evaluation), synthesis methods, and synthetic products.

2. Method
We conducted a literature review of several journals in 2004-2020. Several methods that can
be used in the synthesis of Al2O3 can be seen in Table 1. It shows that Al2O3 can be synthesized
through precipitation, combustion, sol-gel, wet chemical, supercritical water synthesis, microwave,
and mechanochemical methods.
Table 1. Method Material Result Advantage Disadvantage Refs
Precipitation Al(NO3)3.9H2O, γ-Al2O3 nanoparticles have a The synthesis method used The synthesis [13]
Methods, materials, Na2CO3, and deionized spherical shape, a size of 4.0- is simple. The product has a process takes a
results, advantages, water. 4.5 nm, a surface area of ~220 high surface area, surface long time.
disadvantages of the m2/g, an average pore acidity, better crystallinity,
synthesis of Al2O3 diameter of 7.0 nm, and a and has high performance
pore volume of ~0.487 ccm3/g. as a catalyst.
AlCl3·6H2O, NH3·H2O, γ-Al2O3 nanoparticles are 5-9 The synthesis process is low The particles have [14]
and C2H5OH (95%). nm in size and have a surface cost and without pollution. heavy aggregation
area of 204-102 m2/g. and the
precipitate cannot
be filtered easily.
Al(NO3)3.9H2O, The diameters of α-Al2O3 The synthesis method used A long time is [15]
Al2(SO4)3.18H2O, particles obtained from Al3+ is simple. The synthesized required for the
CO(NH2)2, and aquades. concentrations of 10 mmol/L particles have high chemical synthesis process.
and 0.5 mmol/L were 200-500 stability, high thermal
nm and 40-70 nm, stability, and fine particle
respectively. The pore size of size.
the α-Al2O3 particles with a
particle size of 40-70 nm,
approximately 6-14 nm.
AlCl3·6H2O, Al powder, The Al2O3 nanopowder has a The synthesis method used The synthesis [16]
HCl, and NH4OH. size of 30-95 nm and is round is simple and the raw process takes a
in shape. materials used are long time.
economical.
Al(N(CH3)2)3 and NH3 Pure 𝛾-Al2O3 nanopowder is 6- The synthesis method used The synthesis [17]
(25 wt %) 24 nm in size, has a surface is simple and economical. process takes a
area of 109-367 m2/g, and has The synthesized product has long time
an almost spherical high quality/purity, as well
morphology. as a high surface area.

Sodium aluminate The average pore size is 12.9 The synthesis method used is The process of [18]
solution, HNO3 nm, pore volume is 0.37 simple, and the cost of formation of the
solution NH4NO3 cm3/g, BET surface area is 86 primary materials is cheap. precipitate must
solution, and ethanol. 86 m2/g. Synthetic products with large be under the
surface area, large volume, required pH.
good resistance, high purity
and can be applied in the
catalytic, adsorption, and
separation fields.
Al2(SO4)3.18H2O, Nearly spherical γ-Al2O This synthesis method can A long time is [19]
Al(NO3)3.9H2O, nanoparticles with the ratio of control the particle size to required for the
distilled water, n(SO42-) to n(NO3-) are 2:8, 3:7, be produced. synthesis process.
polyethylene glycol 4:6, and 5:5. The average
6000, and particle size of γ-Al₂O₃ is 23, 39,
polyethylene glycol 5, 41.5, and 45 nm. Their
200. particle size distributions are 11-
37, 27-51, 27-60.5, and 29-61
nm, respectively.
Al2(SO4)3.18H2O, Mesoporous Al2O3 with surface The synthesized product has The synthesis [20]
water, NH3.H2O (1,56 area (412 m2/g), pore volume high thermal stability and process takes a
wt.%), and anhydrous (2.3 cm3/g), pore diameter (19.2 high surface area. long time
ethanol. nm), and high thermal stability
(up to 1000°C).

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 Adzra Zahra Ziva, et al.

Method Material Result Advantage Disadvantage Refs

Al2(SO4)3. 18H2O Al2O3 particles with an average The method used is simple The synthesis [21]
(99,9%), AlCl3 (99,9%), size of 0.4 m and round in and has the potential to process takes a
distilled water, urea shape. Particles with a produce spherical ultrafine long time
(99%), tween80 (99%), spherical degree of 1.1 and a Al2O3 particles that can be
sodium stearate (99,8%) size of 0.36 micrometers were applied in the preparation
surfactant, NaCl (99,9%), obtained when the optimum of other spherical oxide
ethanol, and AgNO3 0,1 concentrations were 0.75 wt.% powders.
M. and 0.14 wt.%, respectively.

Al(NO3)3·9H2O (95%), γ-Al2O3 powders which have a γ-Al2O3 powders have high A long time is [22]
NH4HCO3 (98%), narrow size distribution of purity. required for the
deionization water, spherical nano-sized particles, synthesis process.
HNO3, NaOH, ethanol, with a surface area of ~140–
andaseton. Precipitating 190 γ-Al2O3, a crystal size of 4-
agent: Na2CO3 (98%), 6 nm, and a pore volume of
NaHCO3 (99,5%), and 0.291–0.467 cm3 g−1
(NH4)2CO3 (99,9%).
Sodium aluminate, γ-Al2O3 nanoparticles contain The synthesized product has The synthesis [23]
carbon dioxide, oxalic impurities, including iron, high purity, high pore process takes a
acid, HG solid calcium, and silicon ions, with volume, and high specific long time. The
desiliconizing agent, a low content of about 0.01%. surface area. synthesized
solid desodium agent I, γ-Al2O3 nanoparticles have a product still
and solid desodium large specific surface area and contains
agent II. high pore volume of 269.9 impurities.
m2/g and 0.57 mL/g,
respectively.
NaOH, Al(NO3)3, 5% α-Al2O3 with a size of 30-40 The deposition process It takes a long [24]
Al(OH)3 bonded liquid, nm. occurs very quickly, and the time to go
nano seed of α-Al2O3, aggregation is reduced, through the
2% PEG20000, distilled resulting in much smaller synthesis process.
water, ethanol. particles.
AlCl3.6H2O, liquid Most of the particles are in the The method used is easy, The formation of [25]
ammonia, ethanol range of 30-50 nm. The simple, and cost-effective. a precipitate must
(98%) specific area of the gamma- There is a weight loss of 4- be at the required
alumina nanoparticles is 16.00 6% at about 410 °C, and a pH level.
m2/g and the maximum pore total weight loss of only
size is 4.13 nm. 23% when the temperature
reaches 800°C.
AlCl3.6H2O, polyvinyl- The structure of α-Al2O3 is The analysis was carried out PVP surfactants [26]
pyrrolidone (PVP) rhombohedral. The average without washing and cause the
size of Al2O3 nanoparticles is purification. nanoparticle size
about 20 nm. Increasing the to decrease with
temperature causes the increasing
average particle size to temperature.
decrease from 26 nm to 10
nm. Al2O3 nanoparticles are
spherical in shape and range in
size from 20-50 nm.
Combustion Solid rocket propellant Alumina nanoparticles are Combustion of solid The average [27]
containing 5-15 m produced as aggregates propellants makes it easy to diameter of the
aluminum, 200-400 m consisting of primary particles. produce burnt aluminum particles varies
ammonium perchlorate, The diameter of the primary droplets. greatly for
and binder. particles is in the range of 10- different clusters.
140 nm. The size of the
aggregate varies in the range
of 0.1 to several micrometers.
Extracted Al(OH)3 form Crystalline nanoparticles in the The basic material for Although Al2O3 [28]
local bauxite, and theta Al2O3 phase. The average bauxite is found in nanoparticles were
sugar. size is 15.5 nm. Al2O3 spherical Indonesia. calcined at a
form with an average size of relatively high
30 nm. temperature of
1200 °C, the particle
size (15.5 nm) was
still quite small.
Al(NO3)3.9H2O 99%, The white solid is Al2O3, water Generates a more extensive The SCS method is a [1]
CO(NH2)2 99%, (H2O), nitrogen gas (N2), area when using VCS mode. bit difficult because
nutrient media agar, CO2gas. The size of the it will cause a
ciprofloxacin, and nanoparticles is approximately precipitate when
double distilled water 20 nm. The Eg value is about ammonium
5.25 eV. The area is 36 nm, the carbonate is added
pore volume is 0.01 cm3, with to ammonium
a pore size of 1.3 nm. nitrate.
Al(NO3)3.9H2O and γ-alumina obtained has an Generates a more extensive The SCS method is a [29]
(NH4)2CO3 area of about 300 m2/g and a area when using VCS mode. bit difficult because
size of about 5 nm it will cause a
precipitate when
ammonium
carbonate is added
to ammonium
nitrate.

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Method Material Result Advantage Disadvantage Refs

Sol-Gel Aluminum isopro-poxide γ-Al2O nanoparticles with a The partial sintering particle The process of [30]
(99 wt%), 2-propanol, surface area of 303 m2/g, a size of the prepared sample synthesizing is
propionic acid, nitric pore volume of 0.55 cm3/g, a is lower. The synthesized required a lot of
acid (65 mass%), pore diameter of 7.4 nm, a product has a high catalytic time.
aluminum nitrat crystal size of 4.7 nm, and a activity and better
nonahydrate (98.5 wt%) particle size of 4.9 nm. performance with the non-
potassium bicarbonate, aqueous media sol-gel
distilled water. synthesis method.
Al(NO3)3.9H2O, γ-Al2O3 measuring ~15 nm, The method used is It takes a long [31]
C6H8O7.H2O, deionized which transformed into α- relatively simple, efficient, time to go
water Al2O3 with a size of 75 nm. and cheap raw material through the
synthesis process.
Aluminum iso-propoxide γ-Al2O3 nanoparticles with a The method used is simple. The synthesis [32]
(AIP), 2-propanol (IPA) surface area of 68.7 m2/g, a The product has a high process takes a
andacetic acid(AA), pore volume of 0.62 cm3/g, surface area and high long time
water. and an average pore diameter thermal stability.
of 34.7 nm.
AlCl3·6H2O, Al powder, α-Al2O3 nanoparticles with a The method used is simple The synthesis [33]
HCl. size of 32-100 nm. and the raw material is procedure is quite
cheap. The product has high long.
purity, it can be used as a
starting powder for the
fabrication of bulk alumina
with nano microstructure.
Aluminum chloride γ-Al2O3 averaged about 30 nm Get a high yield of pure The synthesis [34]
(AlCl3), ethyl alcohol for 0.1, 0.15, and 0.2 M AlCl3, nano alumina particles. The process takes a
(C2H5OH), and while the average was about results of the preparation of long time.
ammonium hydroxide 40 nm for 0.25 M AlCl3. alumina particles are about
(NH4OH as 28% 82-85%, the range of results
ammonia solution) is more satisfactory than
the theoretical results.
Al(NO3)3.9H2O, pure The nanoparticles have a Simple and inexpensive. Crystalline forms [12]
water, ethanol. polycrystalline structure and a Does not require have heteroge-
rhombohedral structure. The complicated tools for neous sizes,
average grain size of α-Al2O3 is preparation. different shapes,
about 29 nm. and spherical and
semi-spherical
shapes.
Al(NO3)3 and (NH2)2CO Al2O3 with a size of 4-400 nm. Material which used not too The process takes [35]
N2, CO2, and H2O much a long time.
AlCl3, sucrose The area of Al2O3 is 260,264 Using organic ingredients The process takes [36]
(C12H22O11), or starch m2/g. The average diameter is (sucrose or starch). a long time
(C6H10O5) 6.26 nm.
AlCl3, 25%NH3 solution, Aluminum oxide nanoparticles Quite affordable The process takes [37]
and polyvinyl alcohol measuring 25 nm have a economically. a long time
(PVA) rhombohedral structure.
Al(NO3)3.9H2O, Amorphous structure at Precursors are used, which The process takes [11]
C6H8O7H2O, and sintering temperatures of can control the a long time
deionized water 600°C and 700°C. Sintering at stoichiometry and
800°C changed the amorphous morphology of
structure into γ-alumina nanoparticles well. Provides
crystals with an average high purity and high specific
crystal size of 11.5 nm. At surface area of solid
900°C, the average crystal particles.
growth reached 15.5 nm. At
1100°C and 1200°C, a white
powder of -alumina was
formed with a crystal size of
about 48 nm.
Aluminum α-Al2O like nanoplates with an This synthesis process can The synthesis [38]
Wet nanoparticles with average diameter of about 80 reduce the α-Al2O3 phase procedure is quite
Chemical 99% purity, aluminum nm and a length of about 300– formation temperature by long.
nitrate, distilled water, 500 nm, without about 200°C when
ammonia, dilute reaggregation. compared to traditional wet
hydrochloric acid, chemical methods.
ethanol

Aluminum can, glacial α-Al2O3 nanoparticles with an This method uses raw The process takes [38]
acetic acid, HCl, NaOH, average size of ~55 nm. materials derived from a long time for the
distilled water with recycling aluminum cans, synthesis of
electrical conductivity which are economical and aluminum acetate
~3 micro S/cm. can reduce waste. precursors.
Commercial Al α-Al2O3 nanoparticles with an A fine transition layer is A long time is [40]
nanometer powder average size of 10–20 nm and formed between Al and required for the
(particle size 80–100 resulted in a well-dispersed Al2O3, which can increase synthesis process.
nm, 99% purity), alumina-coated Al composite the bond between Al and
aluminum nitrate (99% with a spherical shape. Al2O3. This method is
purity), HCl, ethanol, suitable for the synthesis of
and ammonia. composite ceramics. Al2O3 -
Al.

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 Adzra Zahra Ziva, et al.

Method Material Result Advantage Disadvantage Refs

AlCl3.6H2O and AACH, which transforms into Adding AlCl3 solution at a The process is [41]
NH4HCO2. Soluble the α-Al2O3 at temperatures of rate of less or more than 1.2 quite long, and
starch, deionized 1150-1100°C, is 20-30 nm in L/h will produce AACH and the nanoparticles
water, and ammonium size. γ-AlOOH so that it will still that accumulate
hydroxide. produce α-Al2O3. are quite a lot.
Synthesis Al(NO3)3.9H2O 99%, The products are γ-Al2O3, The temperature used is Still need further [42]
under and distilled water 18 HNO3, H2O, and γ-AlOOH. relatively low compared to experiment for
supercritical ohm. other methods, and the dispersing agent
water results obtained are pretty
conditions small.
Microwave Aluminum Nitrate All nanoparticles appear to Microwave radiation can be The nanoparticles [43]
(>98%), plant extracts have a nearly spherical shape. used as a powerful heat are significantly
(Syzygium aromaticum, The nanoparticle clusters are source for the synthesis of smaller than the
Origanum vulgare, between 60-300 nm. nanoparticles from the dimensions
Origanum majorana, liquid phase in a short time. estimated from
Theobroma cacao, and the SEM images,
Cichorium intybus), which may be
ethanol rooted in the
agglomeration of
the nanoparticles.
Mechano- AlCl3.6H2O and AACH, which transforms into Compared with the wet The pH must be [41]
chemical NH4HCO3. Soluble α-Al2O3 at the temperature of chemical method, this maintained at 9-
starch, deionized 1150-1100°C, is 30-40 nm in method is simpler, the 10 by adding
water, and ammonium size. calcination temperature is ammonium
hydroxide. lower, and the resulting hydroxide.
nanoparticles are less
agglomerated, making them
more suitable for
commercial manufacture.
Fe2O3 and Al Al2O3 with a size of 12 nm and This mechanochemical The pH must be [44]
Fe method requires low maintained at 9-
manufacturing costs for 10 by adding
large quantities ammonium
hydroxide.
Hydrolysis Aluminum phosphide γ-Al2O3 nanoparticles with a The synthesized product has A long time is [45]
powder (>85%), surface area of 285 m2/g. high thermal stability. required for the
deionized water. synthesis process.

3. Results and Discussion

Based on the reviewed studies, several general methods for synthesizing Al2O3 include
precipitation, combustion, sol-gel, wet chemical, supercritical water synthesis, microwave,
mechanochemical, and hydrolysis. The methods and results of several studies will be discussed
below.

3.1. Precipitation method

Precipitation is the most common method for the synthesis of Al 2O3 nanoparticles because
this method is the simplest [13]-[23], low raw material cost [16]-[18], and without pollution [14].
The precipitation method has several advantages, such as high purity products [17], [18], [22], [23],
high thermal stability [15,20], nearly homogeneous nanoparticles in size [25], and control the
desired particle size [19]. The precipitation method forms a solution as a phase transition of
alumina [17]. The pH and temperature of the solution in the formation process are critical for this
method.
The starting materials used in this method are Al(NO 3)3.9H2O, Al(NO3)3.9H2O, CO(NH2)2,
anhydrous alcohol, and distilled water. These ingredients are weighed and measured in
stoichiometric ratios. The solution was made by dissolving the reagents Al(NO3)3.9H2O and
Al2(SO4)3.18H2O into distilled water. After that, CO(NH2)2 is added to the solution, and the solution
mixture is heated to 95°C. Then, the resulting Al(OH)3 precipitate was washed and dried at 60°C.
After that, the product was calcined for 2 hours and cooled at room temperature [15].
The synthesis results showed that the Al(OH)3 particles formed from the aggregation of small
primary colloids would experience particle shrinkage, increasing pore size during the calcination
process. X-ray diffraction (XRD) using an X-ray diffractometer (Rigaku D/max-2400, Japan) with Cu
Kα radiation (40 kV, 60 mA) in the 2𝜃 range of 10°–80° was used to study the crystal structures of
the samples. The measurement was carried out at a 5°/min scan rate with a 0.02° step size. Based
on XRD analysis, during the calcination process of Al(OH)3 particles, a phase transformation
occurred with the amorphous sequence Al(OH)3 → γ-Al2O3 → α-Al2O3. Figure 1 presented the X-ray
Diffraction (XRD) pattern of Al(OH)3 particles calcined at different temperatures for 2 hours. A field-

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 Adzra Zahra Ziva, et al.

emission scanning electron microscope (SEM,

Hitachi S-4800, Tokyo, Japan) was used to
investigate the morphologies of the samples at
a voltage of 15 kV. The SEM analysis shows the
particles have monodisperse and spherical
shapes. Figure 2 shows an SEM micrograph of
α-Al2O3 particles obtained from calcining
Al(OH)3 at 1200ºC for 2 hours. The diameters
of α-Al2O3 particles obtained from Al3+
concentrations of 10 mmol/L and 0.5 mmol/L
were 200-500 nm and 40-70 nm, respectively.
Figure 1. The diameter of these particles can be changed
XRD pattern of sample by adjusting the concentration of Al3+ in the
calcined results [15] solution. The higher the Al3+ concentration
shows the larger particle diameter [15].
This synthesis uses starting materials,
namely sodium aluminate solution, HNO3
solution, NH4NO3 solution, and ethanol. These
ingredients are weighed and measured in
stoichiometric ratios. The sodium aluminate
solution is pumped into the HNO3 solution at
30°C. Then, the white precipitate was covered
(sealed with PE film), reacted at 30°C, and
ripened at 60°C. After ripened, the colloid was
filtered and washed with a solution of NH4NO3
Figure 2. and ethanol. Afterward, the colloid was dried
SEM micrograph of α- at 110°C, calcined to 500°C, and heated at
Al2O3 particles with 500ºC for 4 hours [18].
Al3+concentration (a) 10
XRD pattern of dry boehmite samples
mmol/L and (b) 0.5
mmol/L [15]
obtained at various pH levels is shown in Figure
3. A pure crystalline boehmite phase with an
orthorhombic structure was formed when the
basicity of the reaction solution was elevated
to pH=10, and no impurity peaks were
observed, indicating a high purity product. The
condition of pH=10 and an aging time of 10
hours were chosen as the optimal synthesis
conditions. Figure 4 shows the XRD pattern of
alumina samples calcined at various
Figure 3.
temperatures. The diffraction pattern of the
XRD pattern of
boehmite phase was changed into the γ-Al2O3
precipitates at various pH
levels: a) pH=5, b) pH=6, phase with cubic symmetry at a calcination
c) pH=8, d) pH=10, and e) temperature of 500oC. No significant changes
pH=11 [18] were found in the structure after heat
treatment increased to 700ºC. Increasing the
calcination temperature up to 900ºC displays a
new phase transformation, namely 𝛿-Al2O3.
The formation of the 𝜃-Al2O3 phase with
monoclinic symmetry at a calcination
temperature of 1000°C was confirmed by
fourier transform infrared (FTIR)
measurements. The SEM micrographs of γ-
Al2O3 particles calcined at 500ºC with a size of
Figure 4.
XRD pattern of calcined
200-100 nm and 𝜃-Al2O3 particles calcined at
precipitate at(a) 500°C, 1000°C with a size of 100 nm were shown in
(b) 700°C, (c) 900°C, and Figure 5 [18].
(d) 1000°C temperatures
[18]

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Gamma-alumina nanoparticles synthesized through the

method of precipitation in water. AlCl 3.6H2O was dissolved in
deionized water and Tween-80 (polyoxyethylene sorbitan
monooleate) was added to the solution as a surfactant. Then,
as a precipitating agent, a solution of formamide in water is
added dropwise to the mixture. The presence of a white
gelatin precipitate shows that Al(OH)3 has formed. This
precipitate was filtered and washed numerous times with
ethanol and water. After drying, the white gel was calcined for
5 hours in the air in a muffle furnace at 550°C, converting
Al(OH)3 into Al2O3 nanoparticles. These ingredients are
weighed and measured in stoichiometric ratios [25].
The formation of alumina nanoparticles occurs in 2
stages, the nucleation stage, and the formation of
nanoparticles. Tween-80 is dispersed in water as a spherical
Figure 5.
nuclear-shell micellar structure with a core of C-C hydrophobic
SEM of alumina
powder after being
chains and a shell of polar –OH groups. Formamide (HCONH2)
calcined at: a) plays an important role in the formation of nanoparticles by
500°C and b) decomposing to produce OH-ions in water which react with
1000°C [18] Al3+ ions to form Al(OH)3 and precipitation occur after the pH
value of the solution reaches the required level. Alumina
nanoparticles are formed when Al(OH)3 is calcined in an inert environment. The schematic of the
synthesis of Al2O3 nanoparticles is shown in Figure 6 [25].
Ali et al. [25] reported nanoparticle morphology determined by SEM and Transmission
electron microscopy (TEM) analysis (Figure 7 and Figure 8). The majority of the particles were in the
30-50 nm range, according to scanning electron microscopy (SEM) analysis. The size distribution
also confirms that most of the nanoparticles are nearly homogeneous in size and proportions. The
energy dispersive X-ray (EDX) element mapping (Figure 9) shows the aromatic structure. These
compounds show great resistance to heat and light, so their degradation requires severe
conditions. According to the Brunauer–Emmett–Teller (BET) method, the gamma-alumina
nanoparticles had a specific area of 16.00 m2/g and a maximum pore size of 4.13 nm.

Figure 6.
Schematic synthesis of
alumina nanoparticle
formation [25]

Figure 7.
SEM images of
nanoparticles: (a) in the
presence of Tween-80 and
formamide, (b) without
Tween-80, and (c) without
formamide. The inset in (A)
depicts the size distribution
of the nanoparticles [25]

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Figure 8.
TEM images of
nanoparticles: (a) in the
presence of Tween-80 and
formamide, (b) without
Tween-80, and (c) without
formamide [25]

Figure 9.
(A) Mapping of EDX
elements and (B)
EDX spectra of
nanoparticles [25]

3.2. Combustion method

The SCS (Solution Combustion Synthesis) process is a self-contained chemical complex that
requires a homogeneous precursor solution. SCS begins with the dehydration and decomposition
of a homogeneous solution and involves many exothermic reactions that produce at least one solid
and a considerable volume of gas [46]. Kandil et al. [47] stated that this method is inexpensive,
convenient, and economical.
Syarif et al. [28] synthesize Al2O3 nanoparticles using the self-combustion method from
bauxite using sugar as fuel. Al(OH)3 is extracted from local bauxite. Al(OH)3 powder is put into a
beaker filled with water. Pour some sugar into a beaker until it is completely dissolved. The mixture
forms a sol. The ratio of Al(OH)3 with sugar is 1:1. To make a gel, the sol is heated to 150°C. The gel
self-combusted at 450°C and was heated for 10 minutes at 600°C. After that, the material was
calcined for an hour at 1200°C to form Al2O3 nanoparticles.
The results of the synthesis of Al2O3 Syarif et al. [28] show crystal nanoparticles in the theta
Al2O3 phase. This shows the role of sugar in inhibiting the formation of the alpha phase during
calcination. The sugar utilized binds Al ions, requiring a calcination temperature of more than
1200°C and a period of more than 1 hour to generate the alpha-alumina phase. According to the
Debye Scherrer method of XRD pattern calculation, the average size is 15.5 nm (Figure 10). Although
Al2O3 nanoparticles were calcined at a relatively high temperature of 1200°C, the particle size (15.5
nm) was still quite small. The TEM image shows the spherical shape of Al 2O3 with an average size
of 30 nm (Figure 11).
Afruz & Tafreshi [29] synthesized
γ-Al2O3 nanoparticles using the
combustion method and ammonium
Figure 10. carbonate catalyst. The combustion
XRD pattern of Al(OH)3 methods used are solid-state
extract from local bauxite combustion (SSC) and solution
and Al2O3 nanoparticles combustion state (SCS). The materials
synthesized using self- used in all types of combustion are
combustion with sugar as
Al(NO)3.9H2O and (NH4)2CO3. So,
fuel calcined at 1200°C for
1 hour [28] expect a reaction is presented in
Equation (1).

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2Al(NO3)3.9H2O + 5(NH4)2CO3 → Al2O3(s) + 8N2(g) + 38H2O(g) + 5CO2(g) (1)

The solid-state combustion method is carried out using the

volume combustion synthesis (VCS) mode. It can produce nano
size with a high area and requires a weak exothermic reaction
that requires activation by pre-heating or an electric field. This
method is done by mixing the ingredients by grinding in a mortar,
and then it will form water, emit CO2, and dry quickly [29].
Solution combustion synthesis (SCS) is a process that
combines combustion with the solution. An exothermic chemical
reaction between the salt and the required metal and organic
fuel is used in this approach. When ammonium carbonate is
added to aluminum nitrate, a precipitate forms, this procedure
Figure 11. is complicated. As a result, this procedure is split into two parts:
TEM image of Al2O3 gel combustion synthesis and traditional VSC [29].
nanoparticles. The
Different results are produced due to the comparison of
average particle size is
30 nm [28]
various combustion modes by Afruz & Tafreshi [29]. The XRD
pattern shows that the same sample has an incomplete structure
in sample d-1 compared to other samples (Figure 12). Alumina has an area above 300-400 m2/g, but
the pore size is often wide, even bimodal (Figure 13), and the fine crystal size is about 5 nm (Figure
14 and Figure 15). This experiment shows that using VCS mode in SCS to synthesize Al 2O3
nanoparticles can produce a higher and specific area than solid combustion.

Figure 12. TEM image of Al2O3 Figure 13. Distribution of the pore sizes in the
nanoparticles. The average XRD pattern on synthesized powder from the MP Plot [29]
synthetic powders prepared by different
combustion modes [29]

Figure 14. TEM of one of the samples [29] Figure 15. Particle size distribution and synthetic powder [29]

3.3. Sol-Gel method

The sol-gel method is a simple and effective method for synthesizing Al2O3 nanoparticles. The
most obviously difference in this method compared to the precipitation method is that the
precipitate is converted into a sol and a gel first. Low synthesis temperature [30],[31],[48]; low raw
material cost [31],[33]; high thermal stability [32]; high purity [48]; and high surface area [32] are
some of the benefits of the sol-gel method.
The raw materials for this synthesis are Al(NO3)3 and C6H8O7.H2O. The stoichiometric ratios of
these ingredients are weighed and measured. Aluminum nitrate and citric acid were dissolved in
deionized water at 60°C until a yellowish sol formed. Next, the yellowish sol is heated to 80℃—

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the viscosity and color of the sol change to a transparent gel. The gel was heated at 200°C, ground
to a fine powder, and calcined [31].
The XRD analysis was used to identify
the nanoparticle phase produced during the
synthesis. The XRD pattern of the
synthesized powder with a C/N ratio of 1.0,
Figure 16. which was calcined at various temperatures,
XRD pattern of the is shown in Figure 16. The characteristic low-
synthesized precursor intensity 𝛾-Al2O3 peak was reached at 800ºC,
(C/N = 1) calcined at indicating the transition from the amorphous
different temperatures
phase to 𝛾-Al2O3. At 950°C, a weak peak of α-
(a) 200°C, (b) 600°C, (c)
800°C, (d) 900°C, (e)
Al2O3 was seen, indicating the transition from
950°C, (f) 1000°C, and (g) the 𝛾- to α-Al2O3 phase. Figure 17 reveals a
1100°C [31] field emission transmission electron
microscope (FETEM) micrograph with a
citrate precursor ratio of C/N = 1.0. The
amount of α-Al2O3 increased dramatically
Figure 17. when the calcination temperature was above
FETEM micrograph of 1000ºC. The XRD pattern of powders
the synthesized obtained from various precursor ratios and
precursor (C/N = 1) calcined at 1000°C is shown in Figure 18. The
calcined at (a) 950°C α-Al2O3 XRD pattern profile became sharper
and (b) 1000°C [31] as the C/N mole ratio increased, with the
characteristic peak of 𝛾-Al2O3 weakening and
disappearing. Figure 19 shows the SEM
micrograph created at 1000ºC calcination.
The calcined Al2O3 powder from C/N = 0.5
shows many plate-like flake structures and
mixed multi-modal crystallites in Figure 19(a).
Meanwhile, as shown in Figure 19(b), the
mole ratio of C/N = 2.0 exhibits severe
Figure 18.
agglomeration. The molar ratio of C/N = 1
XRD pattern of α-Al2O3
yielded relatively good results with α-Al2O3
calcined at 1000°C (a) C/N =
0.5; (b) C/N = 1.0; and (c) ultrafine powder with a particle size of 200
C/N = 2.0 [31] nm, according to the results of the study [31].
Mohamad et al. [11] synthesized
alumina nanoparticles by sol-gel method
using aluminum nitrate ((Al(NO3)3.9H2O),
citric acid (C6H8O7H2O), and deionized water.
These materials were weighed and measured
in stoichiometric ratios. Aluminum nitrate
Figure 19.
was dissolved with citric acid in deionized
FETEM micrograph of α-
Al2O3 calcined at 1000°C
water. The solution was stirred at 60°C until
(a) C/N = 0.5 and (b) C/N it turned into a yellowish sol. The solution
= 2.0 [31] was then heated to 80°C and stirred
constantly until a transparent gel was
formed. In an oven, the gel was dried at 90°C.
The dry gel was ground and sintered at
various temperatures, such as 600°C, 700°C,
800°C, 900°C, 1000°C, 1100°C, and 1200°C.
The results of the synthesis showed that
only samples were sintered at temperatures
of 1000°C, 1100°C, and 1200°C which turned
Figure 20. into a white powder. Sintering at
XRD pattern of synthesized
temperatures below 1000°C produces a black
and heat-treated samples
at: (a) 1200°C, (b) 1100°C, powder. The residual carbon inherited from
(c) 1000°C, (d) 900°C, (e) the sol that is not completely burnt is
800°C, (f) 700°C, and (g) assumed to be responsible for the
600°C [11] appearance of black powder. The amorphous

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structure obtained for the powders sintered at 600°C and 700°C can be seen in the XRD pattern
(Figure 20). When the sintering temperature was increased to 800°C, it showed a transition from
the amorphous structure to the γ-alumina phase. At 900°C, the production of γ-alumina becomes
more intense. Alumina begins to grow when the temperature reaches 1000°C. At 1100°C, the
transition from γ-alumina to α-alumina is complete. The α-alumina phase does not change at a
sintering temperature of 1200°C. At sintering temperatures of 600°C and 700°C, due to the
amorphous structure, no crystal size can be determined. The average crystal size for those sintered
at 800°C is 11.5 nm. When the temperature was increased to 900°C, the average crystal growth
reached 15.5 nm and this value was not much different from that of the sample sintered at 1000°C
consisting of a mixed alumina phase. Significant crystal growth was seen when the sintering
temperature was increased to 1100°C and 1200°C where the average crystal sizes were 46.6 nm
and 49.1 nm, respectively. Figure 21 shows the SEM micrograph of the nanoparticles [11].

(g) (b)

(c) (d)

(e) (f)

Figure 21.
SEM micrograph of
alumina nanoparticles
sintered at different
temperatures: (a) 0°C,
(b) 600°C, (c) 700°C, (d)
800°C, (e) 900°C, (f)
1000°C, (g) 1100°C, and
(h) 1200°C [11] (g) (h)

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Nayar et al. [35] used aluminum nitrate

(Al(NO3)3) and urea ((NH2)2CO) to make Al2O3
nanoparticles. Aluminum nitrate and urea
are dissolved in distilled water to make sol.
This sol is heated to 70-80°C in a stirring
position on a hot plate for 4-5 hours, yielding
a translucent and colorless gel. At a specific
time, the gel is immersed in a bath with a
temperature of 450-600°C. As a result, the
reaction's formula is presented in Equation
Figure 22. (2).
Micrograph XRD of
2Al(NO3)3 + 5(NH2)2CO → Al2O3 + 8N2 + 8CO2
nanoparticles prepared
by the SGAC method [35] + 10H2O (2)
The results obtained by Nayar et al.
[35] is a crystal size 44.42 nm. The regular
decomposition of aluminum nitrate and urea
helps obtain alpha-alumina nanoparticles at
a relatively low temperature compared to
the non-fuel synthesis, periodically
converted to alpha at 1100oC.
Figure 22 presented the XRD
diffractogram for the nanoparticles. Samples
Figure 23. that are heated at high temperatures have
SEM micrograph of the same XRD pattern as alpha-alumina in
nanoparticles using the the irreversible phase. Figure 23 shows the
SGAC method [35] SEM image of the alumina morphology with
the calcination temperature increasing from
800 to 1100oC. Figure 24 depicts the
thermogravimetric Analysis (TGA) of all
samples and their mass loss comparisons
based on increasing temperature.

Figure 24.
TGA of alumina powder
prepared by chemical
precipitation (CP) and sol-
gel auto combustion
techniques (S-5) [35]

3.4. Wet chemical method

The Al2O3 nanoparticles were successfully synthesized by the wet chemical method. In this
method, the precipitate formed is obtained by dropping the precipitate into the solution at a
specific rate. The pH of the solution strongly influences this method. The wet chemical has several
advantages, including raw materials derived from waste recycling [38], the resulting product has a
uniform size and high thermal stability [39].
Aluminum nanoparticles (100 nm) with 99% purity, aluminum nitrate, distilled water,
ammonia, dilute hydrochloric acid, and ethanol are used as starting materials in this method. The
synthesis process is depicted in Figure 25 in the flow diagram. In stoichiometric ratios, these
materials are weighed and measured. First, distilled water is used to dissolve aluminum nitrate.
Then, aluminum nanopowder was added, and ammonia was dripped into the mixture at a speed
of 100 drops/minute. To prevent aggregation, dilute hydrochloric acid is added. The pH value of
the solutions was maintained at 6, throughout the reaction. The composite deposit was filtered
and washed with distilled water or ethanol. Next, the precipitate obtained was dried at 80°C and
calcined to 1100°C [38].

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The precursor phase before and

after calcination was determined by
XRD analysis. Figure 26 presented the
synthesized XRD pattern with different
calcination temperatures. The 𝛾-Al2O3
phase was observed after the sample
was calcined at 450°C. Only the 𝛿-Al2O3
phase was observed at a calcination
temperature of 800°C. When the
temperature is raised to 1000°C, the 𝜃-
Al2O3 phase takes over, and when the
temperature is raised to 1100°C, the
complete α-Al2O3 phase is obtained.
Compared to the traditional wet
chemical method, the addition of
aluminum additives reduced the α-
Al2O3 phase formation temperature by
about 200°C. The powder shape and
particle size of the synthesized product
were observed by TEM, as shown in
Figure 27. The TEM observations verified
Figure 25. that the dried boehmite particles
Flowchart of the looked like fibers (Figure 27a). Increasing
synthesis
calcination temperature causes an
procedure [38]
increase in particle size, and its shape
becomes like a plate. These plate-like
Al2O3 grains have a mean diameter of
about 80 nm and a length of about 300-
500 nm, without reaggregation, as
shown in Figure 27d [38].
The starting materials for this
synthesis were aluminum cans, glacial
acetic acid, HCl, NaOH, and distilled
water with a conductivity of ~3 𝜇S/cm.
Stoichiometric ratios are used to weigh
and measure these ingredients. First,
the aluminum can was cut to a size of 2
Figure 26.
× 2 cm2, and glacial acetic acid was used
XRD pattern: (a) dry gel,
(b) sintered at 500°C, (c)
to remove the paint and the inner
sintered at 800°C, and (d) covering polymer. Aluminum is
sintered at 1100°C [38] dissolved in two ways: one uses HCl and
the other uses acetic acid. In the first
procedure, aluminum is dissolved into
HCl, and NaOH is added dropwise to
produce aluminum hydroxide. The
precipitate was washed with distilled
water until the electrical conductivity
was below 50 𝜇S/cm in residual water.
Subsequently, the aluminum hydroxide
precipitate was filtered, dried at 90°C,
Figure 27. and treated in the temperature range of
TEM micrograph 900-1160°C. In the second procedure,
of sintered aluminum is dissolved in glacial acetic
boehmite at acid for several days (90-150). Then, the
different white precipitate was centrifuged at
temperatures: (a)
2500 RPM, washed, dried at 90°C, and
dry gel, (b) 500°C,
(c) 800°C, and (d) treated in a temperature range of 900-
1100°C [38] 1160°C [39].

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The crystal structure of the

precursor and calcined powder was
determined by XRD analysis. Figure 28
shows the XRD pattern of aluminum
hydroxide and the results of powder
synthesis after being heat-treated by
the HCl-NaOH route. The aluminum
Figure 28. hydroxide precursor consists of a
XRD pattern of aluminum mixture of Gibbsite (G = Al2O3-3H2O),
hydroxide and heat- Boehmite (Bh = Al2O3-H2O), and
treated powder at Bayerite (By = Al2O3-3H2O, a gibbsite
different temperatures polymorph). Only crystalline powder
for 3 hours (G = Gibbsite, 𝛿-Al2O3 was obtained on the
Bh = Boehmite, and By = aluminum acetate route before
Bayerite) [39]
reaching the α-Al2O3 crystal phase,
according to XRD patterns. The 𝛿-
Al2O3 phase powder was obtained at
900°C using the NaCl-NaOH route,
and a mixture of 𝛿-Al2O3 and 𝜃-Al2O3
phases was obtained at 1000°C.
When the temperature was 1160°C,
Figure 29. the α-Al2O3 phase was formed. The
SEM images of
SEM image shown in Figure 29
precursors: (a) aluminum
acetate, (b) aluminum reveals the morphology of the
hydroxide at 1100ºC for untreated and heat-treated
3 hours, (c)α-Al2O3 from precursors at 1100°C of both
aluminum acetate, and procedures. As shown in Figure 29c
(d)α-Al2O3 from and Figure 29d, the crystal sizes
aluminum hydroxide [39] obtained from the aluminum acetate
and aluminum hydroxide samples after heat treatment at 1100°C were 54 nm and 58 nm,
respectively [39]. This method is a little challenging to do because to dissolve AlCl3 an acidic
condition is needed to react with urea. Still, a relatively alkaline condition is needed when it has
turned into γ-AlOOH or AACH, with a pH value of 8.5-10. α-Al2O3 obtained at a temperature of
1150-1100°C is 20-30 nm in size [41].

3.5. Synthesis under supercritical water conditions method

The supercritical water method is one of the hydrothermal synthesis methods. To control the
morphology of the material using low or high pressure is required depending on the composition
of the reaction required. Using this method will reduce material losses [46]. The disadvantage of
this method is that it results in agglomeration and large secondary particle size [42].
Noguchi et al. [42] used a continuous
flow system of chemicals using the
supercritical water approach. Aluminum
Nitrate (Al(NO3)3.9H2O 99%) and 18 ohms
distilled water are used in this procedure.
The distilled water is placed in a container,
then removed through a high-pressure hose
with a flow rate of 24-43.5 g/min and a
pressure of 25-35 MPa, entering an electric
heater with a temperature of 585, while
Al(NO3)3 is placed in a container and flowed
through a high-pressure hose with a flow
rate of 3.5-20 g/min and a pressure of 25-35
MPa. With hot distilled water, Al(NO3) will
Figure 30. dissolve. A hydrothermal reaction occurs
Schematic diagram when the reactants enter the reactor tube
of a flow reaction at the correct temperature, producing γ-
system [35] Al2O3 or AlOOH (Figure 30).

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In the experiment, Noguchi et al. [35] is the first report for synthesizing 𝛾-Al2O3 at a
temperature of 410℃ or the temperature in supercritical water. The results of 𝛾-Al2O3 from 𝛾-
AlOOH become dominant due to the dehydration reaction resulting from a water density of 0.357-
0.251 g/cm3 with a temperature of only 10°C. The size obtained is at 4-6 nm (Figure 31), depending
on the temperature and reaction time. With increasing reagent concentration and decreasing pH,
the particle size of 𝛾-Al2O3 decreases. With increasing temperature and collection time, the particle
size of 𝛾-Al2O3 also increases.

Figure 31.
TEM image of 𝛾-Al2O3
particles. Reaction
pressure: 30 MPa,
reaction temperature
(°C)–Al(NO3)3·9H2O
concentration (M)–
reaction time (s): (a) 425–
0.1–0.12; (b) 425–0.3–
0.12; (c) 425–0.1–1.2; (d)
450–0.1–3; (e) 500–0.1–
2.6 and (f) 500–0.3–2.6.
Image adapted from
Noguchi et al. [35]

3.6. Microwave method

Microwave radiation can be used as a powerful heat source for the synthesis of nanoparticles
from the liquid phase in a short time [43]. Microwave heating is considered a more efficient way
of controlling heating because it requires less energy than conventional methods. This is due to the
different heating mechanisms. In a microwave oven, the sample is generated within the sample
itself due to the interaction of the microwaves with the material. Meanwhile, in conventional
heating, the heat generated by the heating element is then transferred to the sample surface
[50,51].

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Hasanpoor et al. [43] synthesize Al2O3 nanoparticles using plant extracts by heating using a
microwave. The materials used are Aluminum Nitrate (>98%), plant extracts, and ethanol. The
plants used were Syzygium aromaticum, Origanum vulgare, Origanum majorana, Theobroma
cacao, and Cichorium intybus. Aluminum nitrate (>98%) and plant extracts were mixed in a ratio
of 1:4 by weight and then stirred. LG 850W microwave model No: MS1040SM/00v with a frequency
of 2.45 GHz was used as the heat source and the solution was irradiated for 10 minutes at 610W.
The irradiated solution was centrifuged and washed with ethanol and deionized water. The powder
is dissolved in deionized water and treated with 150W ultrasonic vibration to reduce
agglomeration.
Hasanpoor et al. [43]
reported the results of the
synthesis showed that all the
synthesized nanoparticles
appeared to have an almost
spherical shape. SEM analysis
(Figure 29) shows a cluster of
nanoparticles in the range of 60-
300 nm. The nanoparticles are
significantly smaller than the
dimensions estimated from the
SEM images, which could be due
to nanoparticle aggregation. The
XRD pattern (Figure 33) of the
particles synthesized with
Syzygium aromaticum showed a
semi-crystalline structure while
the others did not show
significant peaks, possibly being
in an amorphous structure. The
nanoparticle size was less than
10 nm according to TEM and
atomic force microscopy (AFM)
Figure 32.
SEM images of
studies, with average sizes of 8,
(a) Syzygium aromaticum, 3, 5, 2, and 9 nm for Syzygium
(b) Origanum vulgare, aromaticum, Origanum vulgare,
(c) Origanum majorana, Origanum majorana, Theobroma
(d) Theobroma cacao, and cacao, and Cichorium intybus
(e) Cichorium intybus [43] plants, respectively.

Figure 33.
XRD pattern of alumina
nanoparticles [43]

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3.7. Mechanochemical method

The term "mechanochemical" refers to a chemical approach that employs the use of tools.
The most common machine is ball milling, which grinds the powder to fine particle size and then
mixes it with the mixture. The ground particles in this machine can be composed of glass [52]. Due
to particle size reduction, intensive grinding increases the exterior contact area between reactant
powders, allowing new surfaces to make contact [44]. Mechanochemical’s advantages are useful
for large-scale production, high purity, and cost-effective [53,54]. The disadvantages of
mechanochemical are required high energy, long period of milling time, contamination of powder
due steel balls, and susceptible microstructure can be grinded [55].
Gao et al. [41] reported on the mechanochemical production of α-Al2O3. AlCl3.6H2O and
NH4HCO3, deionized water, and ammonium hydroxide were employed. The mixture of 0.03 moles
of AlCl3.6H2O and 0.15 moles of NH4HCO3 is ground. After that, 20 mL of ammonium hydroxide
solution (25%) was added and crushed. The pH of the final product will be 9-10. Deionized water
and ethanol were used to filter and wash the precursors, respectively. Together with the precursor,
the soluble starch was weighed and dispersed in anhydrous ethanol. After 30 minutes of
sonication, the mixture was filtered and dried at 60°C for 30 minutes. The dry mixture was calcined
for 1.5 hours at 1100°C in an air environment.
In this method, the pH must be
maintained to a value of 9-10 by
adding ammonium hydroxide.
Compared with the wet chemical
method, this method is simpler, has
lower calcination temperature, and
results in fewer agglomerated
nanoparticles, making it more
suitable for commercial
manufacture [41].
Figure 34.
XRD pattern of sediment
The results obtained by the
obtained from (a) wet- research of Gao et al. [41] for this
chemical and (b) method, AACH is transformed into
mechanochemical α-Al2O3 at a temperature of 1050-
methods [41] 1100°C with a particle size of 30-40
nm. The XRD pattern of the
mechanochemical is shown in Figure
34b. Figure 35 presented TEM
photography of α-Al2O3 powder.
Figure 36 is an SEM image of the α-
Al2O3 powder prepared without and
with starch as the dispersant.
The synthesis of α-Al2O3 by this
approach was also published by
Figure 35.
Bodaghi et al. [37]. This
XRD pattern (a) TEM
photograph of the α- mechanochemical approach,
Al2O3 powder prepared according to the literature, requires
by the mechanochemical cheap manufacturing costs for big
method [41] numbers. Fe2O3 and aluminum are
the materials employed.
Bodaghi et al. [44] produced
the results are α-Al2O3 crystals
measuring 12-20 nm. Ball-milling
yields nanocrystalline materials with
Figure 36. amorphous fractions, and
SEM display of α-Al2O3 microstructures must be considered
powder prepared (a) when employing these materials,
without and (b) with according to the findings. In fact, the
starch as dispersant by process's low temperature causes
the mechanochemical disruption, which leads to
method [41]
amorphization. Kinetics, rather than

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thermodynamics, can dictate the final structure. XRD traces of iron (III) oxide and aluminum from
1 to 100 hours are shown in Figure 37. Figure 38 presented SEM micrographs of milled particles over
time. The TEM sizes are shown in Figure 39 and Figure 40 under various settings. Figure 41 depicts
the high-resolution transmission electron microscopy (HR-TEM) of the powder mixture after 20
hours.

Figure 37.
XRD pattern of the sample
for t=1-100 h [44]

Figure 38.
SEM micrograph (second
electron mode) of α-Al2O3
nanocrystal formed from
the reduction of hematite
under mechanical alloying
for (a) 5h, (b) 10 h, (c) 20 h,
(d) 30 h, and (e) 40 h [44]

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Figure 39.
TEM image of the powder
mixture ground for 20
hours before washing with
HCl [44]

Figure 40.
TEM image of a powder
mixture ground for 20 h
after 20 h with HCl (α-
Al2O3) (a) bright-field TEM
micrograph (b) SADP
association [44]

Figure 41.
HR-TEM image of the
powder mixture for 20 h
after washing with HCl [44]

3.8. Hydrolysis method

One of the methods for synthesizing Al2O3 nanoparticles is hydrolysis, which is based on the
hydrolysis reaction of the raw materials mixed in the reactor and depends on temperature. This
method yields nanoparticles with a large surface area and high thermal stability [45].
This synthesis uses aluminum phosphide powder (>85%) and deionized water as the starting
material. These ingredients are weighed and measured in stoichiometric ratios. First, deionized
water is added to the aluminum phosphide powder in the reactor. The temperature of the reaction
was kept constant at 363 K. After the reaction was completed and cooled to room temperature, a
precipitate of aluminum hydroxide was obtained and filtered, and washed with deionized water.
The PAlOH sample was prepared by drying the filter cake at 373 K for 12 hours, and the PAl-773
sample was prepared by calcining the PAlOH at 773 K for 3 hours [45].
The XRD results of the PAlOH samples calcined at different temperatures are shown in Figure
42. The diffraction pattern of bayerite disappeared after calcination at 773 K. Weak peaks of 𝛾-
Al2O3, and different AlN peaks were observed. The phase, degree of crystallinity, and crystal size
all influence the XRD peak intensity. Perfect crystals and large crystal dimensions lead to high
intensity of characteristic peaks. The intensity of the diffraction peak increases as the calcination
temperature rises, and more other phases appear. The crystallites grew with fewer defects after
being calcined at 1273 K, as evidenced by the increase in the peak intensity of the 𝛾-Al2O3 phase.

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 Adzra Zahra Ziva, et al.

The 𝛾-Al2O3 and 𝜃-Al2O3 phases predominated after 3 hours of calcination at 1473 K, with a minor
α-Al2O3 phase. Figure 43 reveals the morphological change from needle-like to rod-like after
calcination at 1473 K. These nano bars were irregular in shape, with a diameter of 7-8 nm and a
length of 130 nm [45].

Figure 42.
XRD pattern of synthesized
PAl calcined for 3 hours at
(a) 773 K, (b) 1273 K, (c)
1473 K, and (d) 1573 K [45]

Figure 43.
TEM electron micrograph
of calcined PAl synthesized
powder at 1473 K. (a) low
magnification image and
(b) high magnification
image [45]

4. Conclusion
Several methods can be used to synthesize Al2O3, such as (1) precipitation, (2) combustion,
(3) sol-gel, (4) wet chemical, (5) synthesis in supercritical water conditions, (6) microwave, (7)
mechanochemical, and (8) hydrolysis. Precipitation is the most efficient method for synthesizing
Al2O3. It is the simplest compared to other methods, has low raw material costs, produces no
pollution, and has several advantages such as high purity products, nearly homogeneous
nanoparticles in size, excellent thermal conductivity, and controlling desired particle size. Further
research is needed to determine the most effective materials and efficient procedure in using the
precipitation method.

Acknowledgment
We acknowledged Bangdos Universitas Pendidikan Indonesia.

Authors’ Declaration
This research was Authors’ contributions and responsibilities - The authors made substantial contributions to the
supported by: conception and design of the study. The authors took responsibility for data analysis,
interpretation, and discussion of results. The authors read and approved the final manuscript.
Funding - No specific funding statement from the authors
Availability of data and materials - All data are available from the authors.
Competing interests - The authors declare no competing interest.
Additional information – No additional information from the authors

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