MANUFACTURING OF ZNO SEMICONDUCTORS
FROM THE ZN(CH3COO)2•2H2O PRECURSOR
VIA A POLYOL-MEDIATED THERMOLYSIS
PROCESS

FABRICACIÓN DE SEMICONDUCTORES DE ZNO A PARTIR
DEL PRECURSOR ZN(CH3COO)2-2H2O MEDIANTE UN
PROCESO DE TERMÓLISIS MEDIADO POR POLIOL

Gregorio Flores-Carrasco

Technological University of Tecamachalco

Jorge Rodrigo Mora

CINVESTAV-IPN, Solid State Electronics Section 07360 México-México

Carlos Bueno

National Technological of Mexico/IT of Apizaco 90491 Tlaxcala-México

Raquel Ramírez Amador

National Technological of Mexico/IT of Apizaco 90491 Tlaxcala-México

Beatriz Huerta-Flores

National Technological of Mexico/IT of Puebla

María Luisa Juárez Hernández

Technological University of Tecamachalco
pág. 9841
DOI:
https://doi.org/10.37811/cl_rcm.v8i6.15836
Manufacturing of ZnO semiconductors from the
Zn(CH3COO)2•2H2O
precursor
via a Polyol-Mediated Thermolysis Process
Gregorio Flores-Carrasco
1
flcagr@hotmail.com

https://orcid.org/0000
-0002-0204-0589
Technological University of Tecamachalco

75
483 Tecamachalco-Puebla-México
Raquel Ramírez Amador

raquel.ra@apizaco.tecnm.mx

https://orcid.org/0000-000
3-0716-4596
National Technological of Mexico
/IT of Apizaco
90491 Tlaxcala
-México
Jorge Rodrigo Mora

rodrigomora17@gmail.com

https://orcid.org/0000-0002-3031-8365

CINVESTAV-IPN, Solid State Electronics
Section 07360 México-México

Beatriz Huerta-Flores

beatriz.huerta@puebla.tecnm.mx

https://orcid.org/0009
-0001-9510-1503
National Technological of Mexico
/IT of Puebla
72220 Puebla-México

Carlos Bueno

carlos.ba@apizaco.tecnm.mx

https://orcid.org/0000
-0003-3203-5884
National
Technological of Mexico/IT of Apizaco
90491 Tlaxcala
-México
María Luisa Juárez Hernández

rectoria@uttecam.edu.mx

https://orcid.org/0000-0001-9735-01
86
Technological University of Tecamachalco

75483
Tecamachalco-Puebla-México
ABSTRACT

In this work, the instrumentation of a system to manufacture ZnO semiconductors using the Polyol
-
Mediated Thermolysis Process
are reported. The semiconductors manufactured from the
Zn(CH
3COO)2•2H2O precursor have been synthesized in different molar concentrations (0.001 M, 0.01 M,
and 0.1 M), at low temperatures and atmospheric pressure. The structural and morphological characteristics

of the ZnO semiconductors
were studied by X-Ray Diffraction (XRD) and Scanning Electron Microscopy
(SEM). XRD has
been confirmed the manufacturing of the ZnO semiconductors with high crystalline
quality. No other crystalline phases were detected.
The SEM micrographs reveal that the morphology of
the non
-agglomerated quasi-spherical particles (composed of nanometer-sized particles) has been
controlled from the agglomerated particles, when the concentration of 0.001 M to 0.01 M is used,

respectively. When the highest concentration has been used, no aggregation occurs and only tiny p
articles
in the nanosized range are obtained.
As a result, the synthesis route successfully demonstrates the
manufacturing of semiconductors in a single step, in a simple
-strategy process, being of low cost and
scalable
to industrial level.
Keywords
: polyol-mediated thermolysis process, scalable zno production, structural and morphological
characterization

1
Autor principal.
Correspondencia:
flcagr@hotmail.com
pág. 9842
Fabricación de semiconductores de ZnO a partir del precursor
Zn(CH3COO)2-2H2O mediante un proceso de termólisis mediado por poliol

RESUMEN

En este trabajo se presenta la instrumentación de un sistema de fabricación de semiconductores de ZnO
mediante el proceso de termólisis mediada por poliol. Los semiconductores fabricados a partir del precursor
Zn(CH3COO)2-2H2O se han sintetizado en diferentes concentraciones molares (0.001 M, 0.01 M, y 0.1
M), a bajas temperaturas y presión atmosférica. Las características estructurales y morfológicas de los
semiconductores de ZnO se estudiaron mediante difracción de rayos X (DRX) y microscopía electrónica
de barrido (SEM). La DRX ha confirmado la fabricación de los semiconductores de ZnO con alta calidad
cristalina. No se detectaron otras fases cristalinas. Las micrografías SEM revelan que la morfología de las
partículas cuasi esféricas no aglomeradas (compuestas de partículas de tamaño nanométrico) se ha
controlado a partir de las partículas aglomeradas, cuando se ha utilizado la concentración de 0,001 M a 0,01
M, respectivamente. Cuando se ha utilizado la concentración más alta, no se produce agregación y sólo se
obtienen partículas diminutas en el rango de tamaño nanométrico. Como resultado, la ruta de síntesis
demuestra con éxito la fabricación de semiconductores en un solo paso, en un proceso de estrategia simple,
siendo de bajo coste y escalable a nivel industrial.

Palabras clave: proceso de termólisis mediado por poliol, producción escalable de zno, caracterización
estructural y morfológica

Artículo recibido 13 enero 2025

Aceptado para publicación: 19 febrero 2025
pág. 9843
INTRODUC
TION
Zinc
Oxide (ZnO) is a II-VI type-N semiconductor compound with a band gap around 3.37 eV and a
wurtzite
-type crystalline structure as a stable phase at room temperature. It has specific optical, electrical
and thermal properties that are very important for a wid
e range of applications, especially in the field of the
electronic and optoelectronic
. However, currently the interest main focus, both scientific and technological,
has been directed towards obtaining nanostructured materials due to the superior propertie
s they show
compared to bulk materials, promoting the development of various techniques that allow the obtaining of

ultrafine particles
(Ramos-Justicia, et al., 2023).
Due to the different properties and potential applications of ZnO,
the renewed interest in nanostructured
ZnO particles has been driven by their attractive and improved properties (electrical, optical, magnetic and

mechanical), for applications including nanolasers
, ferromagnetic semiconductor nanomaterials,
piezoelectric semiconductor
s, among other (Ramos-Justicia, et al., 2023; Salvador Alcántara, et al., 2008).
Recently, the physical and chemical properties of nanostructured ZnO also make it very attractive for

wastewater treatment, attracting considerable attention due to its photocatalytic property
for the degradation
of various environmental pollutants
(Flores‐Carrasco et al., 2014; Muñoz-Fernandez et al., 2017; Flores‐
Carrasco et al., 2021
, ).
The results discussed above suggest that there are still several problems to be
solved for devices based on
ZnO nano
- and microstructures to reach optimal efficiencies and be truly competitive within the
technological market. Among the fundamental problems is the control of the morphological
and structural
properties of
the ZnO nano- and microstructures in relation to their manufacturing process. Therefore, the
great technological interest aroused by
the ZnO and the existence of points open to study and improvement
in its manufacturing processes, have
been driven the development and interest in the generation of different
synthesis
methodologies. Up till now, the synthesis methods such as: spray pyrolysis (Salvador Alcántara,
et al., 2008; Flores‐Carrasco et al., 2014), hydrothermal (Sierra
-Fernandez et al., 2014), solvothermal
(Muñoz
-Fernandez et al., 2017), vapor-solid (Bueno et al., 2018, Bueno et al., 2024), thermal treatment
(Mora, et al., 2019),
chemical bath deposition (Flores‐Carrasco et al., 2021), and many others, the main
need is the development of a simple process which allows controlling the characteristics of the particles

including the control of size, morphology and chemical c
omposition, in a reproducible way, being of low
pág. 9844
industrial cost, continuous operation and high performance. Taking the above into account, the method that

has managed to achieve these expectations to manufacture functional semiconductors with specific

properties, suitable for new applications, has been
the Polyol method (Martínez-Martínez et al., 2021;
Flores‐Carrasco et al., 2021
).
Due to the approaches already presented, in this work we
re report the instrumentation of a system for the
ZnO semiconductors
manufacture by a Polyol-Mediated Thermolysis Process. Likewise, a systematic study
of the experimental parameters has been carried out during the manufacturing process of
the ZnO
semiconductors, without forgetting the academic challenge of addressing manufacturing aimed at obtaining

nanostructured semiconductor materials, due to the superior properties that these show, as well as contribute

to a greater understanding of the influen
ce of the configuration in the technique used on the morphological
and structural characteristics of the ZnO semiconductors obtained.

METHODOLOGY

Manufacturing synthesis.
As a first step, the stoichiometric amount of Zn(CH3COO)2•2H2O and
Polyvinylpyrrolidone (PVP) was dissolved in Ethylene Glycol (EG) in a three
-necked flask fitted with a
reflux condenser. Figure
1A shows the block diagram of the complete system of the Polyol-Mediated
Thermolysis Process,
employing for the ZnO semiconductors manufacture. Subsequently, the reaction
solution thus obtained was stirred vigorously and then heated to a temperature of 185 °C. The reaction

continued for 2 hours, after which the system was cooled to room temperature. The particles thus obtaine
d
were separated from the liquid by centrifugation and then washed repeatedly with deionized water.
Finally,
the particles were dried into a furnace out at 500 °C in an air atmosphere for 2 hours, and then a white

powder sample of the zinc oxide precursor was collected.

Characterization techniques
. X-Ray Diffraction (XRD) analysis was used to investigate the crystalline
phase and structure of
all the as-synthesized samples. These measurements have been performed on an X-
R
ay Diffractometer (Philips X´pert) with CuKα radiation (λ = 1.5406 Å) and over ther ange 2θ = 25-50° at
room temperature.
To study the morphology of all the as-synthesized samples, Scanning Electron
Microscopy (SEM, FEI Teneo / EDAX
-Dx4) analyses has been carried out employing an accelerating
voltage of 5 kV.
pág. 9845
RESULTS AND DISCUSSION

Figure 1
B shows the XRD patterns of all the ZnO semiconductors manufacture, from the different
concentration in the (0.0
01 M, 0.01 M, and 0.1 M) precursor solution. These patterns present the typical
diffraction peaks that were assigned to the (1 0 0), (0 0 2), (1 0 1), and (1 0 2) planes of the ZnO structure

(JCPDS data card no. 80
-0075). Furthermore, the typical hexagonal (wurtzite) structure of all the ZnO
semiconductors manufacture samples has been inferred from the XRD pattern, which is in good agreement

with the intrinsic fundamental structure of ZnO as reported in the literature
(Ramos-Justicia, et al., 2023;
Flores‐Carrasco et al., 2021
, Bueno et al., 2024). No other crystalline phase was detected. Additional, it has
been found that the intensity of the all peaks improvement with the increase in the concentration of the

precursor solu
tion, indicating that the crystalline quality also improved. Has been observed, also, that the
Full Width Half
-Maximum (FWHM) of the peaks became wider when increase the concentration of the
precursor solution, indicating that the decreases particles sizes.

From the SEM micrographs shown in Figure 1C, has been study the morphology of all the ZnO

semiconductor samples,
independently of the initial reagent concentration used in each experiment. In
Figure
1C(a), can be only observed in the SEM micrographs quasi-spherical particles agglomerated when
the precursor a lower concentration has been used.
In the case of 0.01 M concentration (Figure 1(b)), the
SEM micrographs clearly revealed quasi
-spherical, non-glomerated particles with a good size distribution,
composed
for subunits of nanometer-sized particles. When has been employing concentration of 0.1 M
(Fig
ure 1C(c)), it is possible to distinguish only the formation of monodisperse and dense particles with a
nanometer
-sized.
pág. 9846
Figure 1
: A) Schematic illustration of preparing for ZnO semiconductors. B) X-ray diffractograms of ZnO
semiconductors manufactured in different concentration of precursor solution. C) SEM images of typical

ZnO semiconductors.

CONCLUSIONS

XRD has been confirmed that all the manufactured semiconductors present the intrinsic fundamental

structure of ZnO. The SEM images revealed that using the highest precursor concentration, the aggregation

process does not occur and it is possible to obtain
particles in the nanometric range.
Finally, the instrumented system by a Polyol
-Mediated Thermolysis Process has been shown to successfully
produce ZnO semiconductors in an efficient and reproducible form. What is evident from these findings is

that the morphology and the particle size has
been controlled, to help promote the large-scale production
of these nanomaterials given their properties to allow various applications in subsequent studies.

ACKNOWLEDGEMENTS

This research was supported by the projects
UTTECAM (Technological University of Tecamachalco),
TecNM (
National Technological of Mexico), and CONAHCYT (National Council of Humanities, Sciences,
pág. 9847
and Technologies
)‐Mexico.
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