XXVI International Materials Research Congress

THERMLUMINESCE STUDY OF THE NANOHYDROXYAPATITE

DOPED WITH SILVER NANOPARTICLES BY MICROWAVE METHOD.
L. S. Villaseor Cern1*, H. Lpez Ruiz2, J. A. Arenas Alatorre 3, K. Alemn 2, D. Mendoza Anaya 4 and V. Rodrguez Lugo2

ventura.rl65@gmail.com

Universidad Autnoma del Estado de Hidalgo, Instituto de Ciencias Bsicas e Ingeniera

ABSTRACT
This work focuses on the study of the thermoluminescent (TL) signal of hydroxyapatite (HAp) doped with silver nanoparticles (AgNps) when it is exposed to gamma radiation. Initially, spherical AgNps were synthesized by polyol
method with three different average particle sizes such as 17, 21 and 29 nm, according to scanning electron microscopy (SEM) and UV spectroscopy analysis (UV-vis). Subsequently, pure and AgNps doped HAp was synthesized by
microwave-assisted hydrothermal method by adding 0.5 wt% of pre-synthesized AgNps during the synthesis. The microstructural characterization of AgNps doped HAp was performed using X-ray diffraction techniques (XRD) and
scanning electron microscopy (MEB) which confirms the HAp phase with (211) as its preferential orientation and a fiber-shaped structures were identified with average sizes ~ 28 to 45 nm in diameter, with a length of 50 to 200 nm. TL
intensity of AgNps doped HAp is increased 45% compared to pure HAp, which is corroborated to the increase in the metastable states due to AgNps incorporation. These powders could be considered as a material for its application in
the development of dosimeters to quantify the intensity of the field of ionizing radiation.

Emission of light due to the electron-hole recombination proved by
the thermal treatment, when the material (HAp) is previously
irradiated [1].
HAp is one of the materials more studied for TL properties due to
its structural defects resulting in metastable states which provokes
TL [2].
The TL signal is directly related to the synthesis methods and
structural defects [1].
INTRODUCTION
Defects are caused by addition of impurities such as Ag, Mn
or Mg in Hap [2].
HAp is a biomaterial within the area of medicine due to its
bioactivity. Also presents a thermoluminescent behavior
when it is exposed to gamma irradiation [3].
The Ag nanostructures are of high interest due to their
properties like optical, electrical and etc [4].

METHODS
1.- synthesis of AgNps by polyol method. 2.- synthesis of HAp/AgNps by 3.- Characterization
The synthesis of AgNps was performed by varying the concentration of
microwave-assisted hydrothermal method.
Sample Characteriza-
The synthesis was performed by microwave-assisted hydrothermal method, Synthesis conditions
stabilizer, polyvinylpyrrolidone (PvP 10) as AgNO3: PvP = 1:1, 1:1.5 and name tion
which was developed in the presence of previously synthesized AgNps.
1:2.
The aqueous solution was prepared with initial concentration of 0.10 M 1:1
Polyol method UV-VIS and
AgNps 1:1.5
AgNO3:PVP SEM.
1:2

Microwave-assisted
hydrothermal DRX, SEM
HAp HAp
and TL
T:200C and t:32 min

HAp/1:1 Microwave-assisted
HAp/ hydrothermal DRX, SEM
HAp/1:1.5
AgNps and TL
HAp/1:2 T:200C and t:32 min

RESULTS
A. SILVER NANOPARTICLES B. HYDROXYAPATITE/SILVER NANOPARTICLES
Ultra violet-visible Spectroscopy. X ray Diffraction. Scanning Electron Microscopy analysis.

Surface plasmonic resosnance.
Displacement of the peak to the infrared range.
Growth of the AgNps with increase in the PVP concentration.
All the XRD peaks are associated with HAp structure based on the JCPDS-89-
The preferential morphologies observed are nanorods and nanofibers.
6440 card .
Rods/fibers size decreases with increase in the size of the AgNps incorpo-
A left shift in the crystallographic (211) plane confirms the incorporation of Ag rated into the HAp lattice.
into the HAp lattice structure in all the doping cases.
No additional phases or calcium or phosphate were observed.

Scanning Electron Microscopy analysis

Sample Nanorod dimensions (nm) Nanofibers dimensions (nm)

Diameter Length Diameter Length
HAp 46 75 68 220
HAp/1:1 44 70 45 180
HAp/1:1.5 54 79 28 250
HAp/1:2 34 83 22 150
Table1 . Morphology and dimensions of the HAp/ AgNps.

Thermoluminescence properties
Intensity (a. u.)

Intensity (a. u.)

Spherical morphology, increment in the size of AgNps and decrease in their agglomeration with Temperature (C)
Temperature (C)
an increase in the PVP concentration.
The average particle size around 7, 21 and 29 nm for samples 1:1, 1:1.5 and 1:2, respectively.
The decrease in the agglomeration and increase in the particle size are due to the steric effects
and are proportional to PVP concentration.
Intensity (a. u.)

Sample HAp HAp/1:1 HAp/1:1.5 HAp/1:2

Dose (GY) TL intensity
5 172 179
Temperature (C)
10 101 313 350 Temperature (C)

20 420 197 623 687

TL analysis without and with irradiation at 5, 10, 20 and 40 Gy for all the three samples, namely, HAp/1:1, HAp/1:1.5 and HAp/1:2.
40 873 395 1,329 1,411.8 Increased TL intensity ~45% of the sample HAp/1:2 in compared to pure HAp, which is corroborated to the increase in the metastable
Table 2. Comparison of the Intensity thermoluminescnt signal of HAp/ states due to AgNps incorporation.
AgNps.

CONCLUSIONS REFFERENCES
The aggregation of the AgNps resulted an increase in size and elongation in shape of the [1] A.J.J. Bos, High sensitivity thermoluminescence dosimetry, Nucl. Instruments Methods Phys. Res. B. 184 (2001) 328. doi:10.1016/
S0168-583X(01)00717-0.
HAp nanomaterial.
[2] Mendoza Anaya D. (2002). Sntesis y caracterizacin de sistemas dosimtricos preparados va sol-gel. Tesis doctoral, 18-23.
The Intensity of TL signal incresaed due to the aggregation AgNps into the HAp and the [3] Zhanga, X., & Vecchio, K. (2007). Hydrothermal synthesis of hydroxyapatite rods. Crystal Growth, 133-140.
best thermoluminescent signal obtained were of the sample HAp/1:2 due to the presence of [4] Y.M. Sgibnev, N. V Nikonorov, A.I. Ignatiev, High efficient luminescence of silver clusters in ion-exchanged antimony- doped photo-
higher metastable states. thermo-refractive glasses: Influence of antimony content and heat treatment parameters, (2017). doi:10.1016/j.jlumin.2017.04.028.

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