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Hydrothermal synthesis of doped ZnO and TiO2

nanomaterials: Opportunities for textile
applications

Article in UPB Scientific Bulletin, Series B: Chemistry and Materials Science · January 2014

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U.P.B. Sci. Bull., Series …, Vol. …, Iss. …, 200.. ISSN 1454-2331

HYDROTHERMAL SYNTHESIS OF DOPED ZnO AND TiO2

NANOMATERIALS: OPPORTUNITIES FOR TEXTILE
APPLICATIONS

Ioan Albert TUDOR1, Mirela PETRICEANU2, Radu-Robert PITICESCU3, Cristian PREDESCU4

Hydrothermal method is a versatile method that may be used to obtain doped

TiO2 and ZnO nanostructures with desired properties to be used as stable suspensions
for applications in fabrication of special textiles. XRD spectra revealed TiO2 and ZnO
nanopowders having crystallite sizes of 28 nm and 35 nm, respectively.
Powders consist from slightly agglomerated nanoparticles that can be easily
de-agglomerated and dispersed for application on the textiles surfaces. The strong
negative zeta potential of the powder (-40…-60 mV) shows that stable colloidal
suspensions are formed. The thermal behavior of textiles embedded with these
nanostructured oxides is also improved.

Keywords: hydrothermal, TiO2 and ZnO nanopowders, textile substrate.

1. Introduction
Utilization of nanomaterials to improve the traditional textiles by adding antiseptic,
antifungal or self-cleaning functionalities is a modern trend in special textiles market niche. Anti-
microbial agents are used to prevent undesirable effects in textiles. The first includes the degradation
phenomena like coloring, staining and deterioration of fibers [1-3]. Because of their dye degradation
potential, some fungus can be used for removing dye from textile effluent [4]. The second one
produces unpleasant odor [5-7] and the third effect is the increase of potential health risks [8-10].
TiO2 with rutile structure has the ability to block the UV radiation leaving the visible light
to cross over a thin film. Alternatively TiO2 as anatase has a very strong photo-catalytic activity and
these combinations of properties is important in achieving optimal antibacterial, UV screen and self-
cleaning and anti-stain properties of advanced textiles.
TiO2 exists in three crystalline structures: anatase (tetragonal), rutile (tetragonal) and
brookite (orthorhombic) [11-16]. TiO2 nano-particles have created a new approach for remarkable
applications as an attractive multi-functional material. TiO2 nano-particles have unique properties
such as higher stability, long lasting, safe and broad-spectrum anti-biosis [17-20]. TiO2 nano-
particles have been especially the center of attention for their photo-catalytic activities [21-30]. This
makes TiO2 nano-particles applicable in many fields such as self-cleaning, anti-bacterial agent, UV
protecting agent [31], environmental purification [32], water and air purifier [33,34], gas sensors,
and high efficient solar cell [11,35,36]. The photo-activity property is strongly related to the
structure, micro-structure and the powder purification [10,11,35,36].
Nanostructured ZnO, combines interesting optical, piezoelectric and antiseptic / antifungal
properties. ZnO is an n-type semi-conductor as well as TiO2 [37]. Recently, ZnO has been found
1.PhD. Student at Faculty Science and Engineering of Materials, Politehnica University of
Bucharest, Romania, albert_tudor@yahoo.com.
2. Research Asistent at National R&D Institute for Nonferrous and Rare Metals, Pantelimon, Ilfov,
Romania
3. Senior Researcher at National R&D Institute for Nonferrous and Rare Metals, Pantelimon, Ilfov,
Romania
4. Prof. Dr. Eng. at Faculty Science and Engineering of Materials, Politehnica University of
Bucharest, Romania, predescu@ecomet.pub.ro.
 Ioan Albert Tudor, Mirela Petriceanu, Radu-Robert Piticescu, Cristian Predescu

highly attractive because of its remarkable application potential in solar cells, sensors, displays, gas
sensors, piezoelectric devices, electro-acoustic transducers, photo-diodes and UV light emitting
devices, sun-screens, UV absorbers, anti-reflection coatings, photo-catalysis and catalyst [10, 37-
48].
Their efficiency is strongly dependant on controlled particle sizes (< 100 nm), morphology
(spherical, whiskers, fibers…..), structural features and surface characteristics ZnO has strong
actions on the mono- and multi-cellular organisms. Not yet clarified destructive effects over the
toxins synthesized by organisms.
The photo catalytic effect is more efficient in artificial UV radiation, depending on wave
length (the best results obtained at 380 nm), exposure time, oxide amount and bacteria type.
The “killer” mechanisms of ZnO is due to the controlled release of [OH] radicals and [O2–
] ions, formed in photo catalytic reactions. An important break-through was the obtaining of thin
ZnO films doped with Ag, which may be used for avoiding room contamination.
Many techniques have been used for deposition of high quality ZnO and TiO 2 films such
as physical vapor deposition (PVD), pulsed laser deposition (PLD), anodizing, sputtering and
thermal evaporation [49-57].
The hydrothermal method is suitable for the direct preparation of nanocrystalline oxide
powders, the main advantages being: one step process to produce nanopowders, no thermal
treatment required to obtain crystalline phases, leading to a good compatibility with organic
materials during processing of textiles, low energy and materials consumption, reduced
environmental impact due to working in close vessels without wastes or gas emissions, scalability
to large production capacities.

2. Materials and methods

Obtaining of textile materials embedded with Ag-doped ZnO nanoparticles consisted in the
main technological steps: one step hydrothermal synthesis of doped nanopowders, obtaining of
stable colloidal suspensions based on these powders, embedding the textile substrate by dip coating
and characterization of the material.
For the hydrothermal synthesis of Ag-doped ZnO nanopowders analytical grade zinc nitrate
hexahidrate Zn(NO3)2 x 6H2O and silver nitrate Ag(NO3)2 were used as raw materials while TiCl4
was used as raw materials for obtaining TiO2 nanopowders. Potassium Hydroxide was used as
hydrolysis agent.
The starting water solutions mixed at the programmed dopant ratio were mixed with KOH
solution to reach a pH > 9.0 for complete hydrolysis of metallic cations. The hydrothermal
crystallization was done in Teflon autoclaves in the temperature range 200-2500C. The powder
formed was filtered and washed with distilled water and ethanol to remove soluble impurities and
reducing agglomeration. The powders were re-dispersed in water using ammonium salt of methyl-
methacrylate as stabilizing agent and the dispersion thus obtained were used for impregnation of a
the textile substrates.
Chemical analysis of the products was done by Inductive Coupled Plasma Optical Emission
Spectroscopy and Atomic Adsorption Spectroscopy. The crystalline structure of powders was
characterized using a Brucker D8 Advance XRD apparatus. Data analysis was done with the
software DIFFRACplus XRD Commander for CuKα radiation and the Bragg-Brentano method with
Θ – Θ coupling in vertical configuration. The mean crystallite sizes were calculated from Scherrer
formula
k
dm= (1)
 cos 
where k is a constant,  is the Bragg angle,  is the wave length of the incident XR radiation and 
is the peak width at half height.
 Hydrothermal synthesis of doped ZnO and TiO 2 nanomaterials: opportunities for
textile applications

The particle grain sizes were measured by laser scattering method using a Malvern ZS90
apparatus. The thermal behavior of materials was characterized by DSC method with the help of a
Netzsch Maya F3 system in the temperature range 20-6000C.

3. Results and discussions

The chemical reactions expected to take place in the hydrothermal solutions were estimated
from the evolution of the equilibrium constant with the reaction temperature for different possible
reaction pathways, with the help of HSC 6 software. According to the analysis done, the reaction
for the hydrothermal synthesis of TiO2 and doped Ag-ZnO nanopowders are respectively:

TiCl4 + 4KOH(a) = TiO2 + 4KCl(a) + 2H2O (2)

Zn(NO3)2 + 2AgNO3(a) +4 KOH(a) = ZnO(a) + Ag2O + 4KNO3(a) + 2H2O (3)

Figures 1 and 2 show the typical XRD spectra of TiO2 and ZnO nanopowders nanopowders
obtained by hydrothermal process.
Table 1 and 2 present some important characteristics of TiO2 and ZnO nanopowders
obtained by hydrothermal procedure respectively.

Fig. 1. XRD spectra of hydrothermally synthesized TiO2

 Ioan Albert Tudor, Mirela Petriceanu, Radu-Robert Piticescu, Cristian Predescu

Fig. 2. XRD spectra of hydrothermally synthesized Ag-doped ZnO

Table 1.
Main Characteristics of TiO2 nanopowders
Lattice parameters
Phase composition
Mean size nm/
Concentration a, Å c, Å
(Scherrer)
TiO2/ anatase 92.9% 3.78944 9.49909 28.3
TiO2/rutil 7.1% 9.13 5.17 26.3

Table 2.
Main Characteristics of Ag-doped ZnO nanopowders
Lattice parameters, Mean
Phase Chemical composition, % gr.
Å size nm/
composition
ZnO Zn5(OH)6(CO3)2 Ag2O Ag a c (Scherrer)
97,3 2,3 0,4 1.50 3,2520 5,2097 35

In figure 3 the particle size distribution of TiO2 and Ag-doped ZnO respectively are presented. It
may be observed that powder consist from slightly agglomerated nanoparticles that can be easily de-
agglomerated and dispersed for application on the textiles surfaces.
 Hydrothermal synthesis of doped ZnO and TiO 2 nanomaterials: opportunities for
textile applications

a)

b)

Fig. 3. Particle size distribution of TiO2 (a) and Ag-doped ZnO (b) obtained by
hydrothermal procedure

Figure 4 presents the evolution of zeta potential of Ag-doped ZnO nanoparticles during acid titration
of the zinc solution with addition of ammonium salt of methyl-methacrylate as dispersing agent. The
strong negative zeta potential of the powder shows that stable colloidal suspensions are formed.

Fig. 4. Evolution of zeta potential of stable Ag-doped ZnO colloidal suspensions

The thermal behavior of TiO2 and Ag-doped ZnO nanostructures is presented in the DSC
diagrams from figures 5 and 6.
 Ioan Albert Tudor, Mirela Petriceanu, Radu-Robert Piticescu, Cristian Predescu

DSC /(mW/mg) Cp /(J/(g*K))

exo Peak: 85.6 °C, 1.351 J/(g*K)

1.300
0.2

1.200
[2.2]

0.15

1.100

Peak: 259.9 °C, 1.019 J/(g*K) [2.3]

0.1 1.000
[3]

Area: 33.26 J/g

0.900

0.05

0.800

Area: 23.76 J/g

[2.2] 2-TiO2 11.08.2009.dd5

0 DSC
0.700
[2.3] 2-TiO2 11.08.2009.dd5
DSC
[3] Cp_2-TiO2 11_08_2009_dd5_1_sapphirre 0_5 mm 10_08_2009_dd5_1.md5
Cp [4]
[4] Cp_2-TiO2 11_08_2009_dd5_2_sapphirre 0_5 mm 10_08_2009_dd5_2.md5
Cp
0.600

-0.05

0.0 100.0 200.0 300.0 400.0 500.0

Temperature /°C

Fig. 5. DSC characterization of TiO2 nanostructures

DSC /(mW/mg)
exo Peak: 259.9 °C, 1.737 mW/mg

1.5

1.0 Peak: 439.1 °C, 0.8728 mW/mg

0.5
Area: 61.78 J/g

Area: 169.2 J/g

0.0
Peak: 496.0 °C, -0.3551 mW/mg

[1.1]
Area: 0.7615 J/g
-0.5
100 200 300 400 500
Temperature /°C

Fig. 6. DSC characterization of polyester textiles embedded with Ag-doped ZnO.

The first endothermic peak observed in TiO2 nanostructures embedded in polyester textiles is related
to elimination of adsorbed water while the second large endothermic peak at 260 0C is related to the
elimination of OH groups from the TiO2 lattice. In the case of textiles embedded with Ag-doped
ZnO three endothermic peak are observed. The first from 260 0C is related to the elimination of OH
groups from the ZnO lattice while the peaks from 439 0C and 4960C may be attributed to the
degradation of the textile substrate.
 Hydrothermal synthesis of doped ZnO and TiO 2 nanomaterials: opportunities for
textile applications

4. Conclusions

Implementation of nanomaterials in textiles requires a strong interaction between research, industry

and local agencies due to the complexity of analytical methods to be used in the preparation of
technology transfer steps and funding of specific activities. Hydrothermal method is a versatile
method that may be used to obtain doped TiO2 and ZnO nanostructures with desired properties to
be used as stable suspensions for applications in fabrication of special textiles with antifungal,
antibacterial and photo-catalytic properties. The thermal behavior of textiles embedded with these
nanostructured oxides is also improved.

5. Acknowledgement
The research was supported from the Contract 7-073/2013 MANUCOAT financed by
UEFISCDI and COST Action MP 1105 Flartex financed by European Scientific Foundation.

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