Scientia et Technica Año XXVI, Vol. 26, No. 04, diciembre de 2021. Universidad Tecnológica de Pereira. ISSN 0122-1701 y ISSN-e: 2344-7214
525
Abstract— In this article, the study of the influence of the
calcination temperature on the crystallographic, compositional,
and morphological properties of the natural hydroxyapatite
taken from sheep bones was carried out. The obtained samples
were characterized by thermogravimetric analysis (TGA), X-ray
diffraction (XRD), Fourier transform infrared spectroscopy (FT-
IR) and scanning electron microscopy, with elemental analysis
(SEM-EDS) in order to obtain structural information,
compositional and morphological properties. In the
thermogravimetric curves, the decomposition temperatures of
the organic phases present in the sheep bones powder were
identified. In the X-ray diffraction analyzes, it was found that the
diffraction patterns presented characteristic peaks of
hydroxyapatite and, it was observed that the increase in
temperature favors the growth crystallite size. Likewise, in the
morphological analysis, changes in the samples were verified,
finding greater agglomeration of the particles, while the EDS
analyzes revealed the different Ca/P relationships for the
calcination temperatures used. In the FTIR spectra, the
This manuscript was sent on June 01, 2021 and accepted on November 26,
2021.This paper is a result of the work developed under the Project “Programa
De Investigación Reconstrucción Del Tejido Social En Zonas De POS-
conflicto en Colombia”, code SIGP: 57579 with the research “Competencias
Empresariales y de Innovación para el Desarrollo Económico y la Inclusión
Productiva de las regiones afectadas por el Conflicto Colombiano” code
SIGP: 58907. Financied by the Colombia Científica call, contract No
FP44842-213-2018.
V.Restrepo-Ramírez is with Universidad Tecnológica de Pereira, Carrera
27 #10-02 Barrio Alamos - Pereira - Risaralda - Colombia (e-mail:
valrestrepor@utp.edu.co)
I. D. Arellano-Ramírez is with Universidad Tecnológica de Pereira,
Carrera 27 #10-02 Barrio Alamos - Pereira - Risaralda - Colombia (e-mail:
arellano@utp.edu.co)
N. Alzate-Acevedo is with Universidad Nacional de Colombia, sede
Manizales, Km 9 via al aeropuerto la Nubia (e-mail: nalzatea@unal.edu.co)
E. Restrepo-Parra is with Universidad Nacional de Colombia, sede
Manizales, Km 9 via al aeropuerto la Nubia (e-mail:
erestrepopa@unal.edu.co)
C.D. Acosta-Medina is with Universidad Nacional de Colombia, sede
Manizales, Km 9 via al aeropuerto la Nubia (e-mail: cdacostam@unal.edu.co)
characteristic vibrational bands of the phosphate and hydroxyl
functional groups present in the samples were observed.
Moreover, due to the temperature changes, the vibrational bands
corresponding to water and proteins disappeared, and a decrease
in the carbonate bands was also identified.
Index Terms— Calcination temperature, FT-IR, hydroxyapatite,
scanning electron microscopy, sheep bone, thermogravimetry, X-
ray diffraction.
Resumen—En este artículo se estudió la influencia de la
temperatura de calcinación en las propiedades cristalográficas,
composicionales y morfológicas de la hidroxiapatita natural
obtenida a partir del hueso de ovino. Las muestras fueron
caracterizadas mediante análisis termogravimétrico (TGA),
difracción de rayos X (DRX), espectroscopia infrarroja por
transformada de Fourier (FT-IR) y microscopia electrónica de
barrido con análisis elemental (SEM-EDS) con el propósito de
obtener información estructural, composicional y morfológica.
En la curva termogravimétrica se identificaron las temperaturas
de descomposición de las fases orgánicas presentes en el polvo de
hueso ovino. En los análisis de difracción de rayos X se encontró
que los patrones de difracción presentan picos característicos de
la hidroxiapatita y que el incremento de la temperatura favorece
el crecimiento del cristal y su tamaño. Así mismo, en el análisis
morfológico se comprobó dichos cambios en las muestras,
encontrando mayor aglomeración de las partículas, mientras que
los análisis EDS revelaron las diferentes relaciones Ca/P para las
temperaturas de calcinación empleadas. En los espectros FTIR,
se observaron las bandas vibracionales características de los
grupos funcionales fosfato e hidroxilo presentes en las muestras.
Además, debido al cambio en las temperaturas, desaparecen las
bandas vibracionales correspondientes al agua y las proteínas y,
disminución en las bandas de los carbonatos
Palabras claves— Difracción de rayos X, FTIR, hidroxiapatita;
hueso de oveja, microscopio electrónico de barrido, temperatura
de calcinación, termogravimetría.
Influence of the Calcination Temperature on the
Crystallographic, Compositional and Morphological
Properties of Natural Hydroxyapatite Obtained from
Sheep Bones
Influencia de la temperatura de calcinación en las propiedades cristalográficas,
composicionales y morfológicas de la hidroxiapatita natural obtenida de huesos de oveja
eweweweewe
V. Restrepo-Ramírez ; I. D. Arellano-Ramírez ; N. Alzate-Acevedo ; E. Restrepo-Parra ;
C.D. Acosta-Medina
DOI: https://doi.org/10.22517/23447214.24888
Artículo de investigación científica y tecnológica
Scientia et Technica Año XXVI, Vol. 26, No. 04, diciembre de 2021. Universidad Tecnológica de Pereira
526
I. INTRODUCTION
N the last 50 years, the diversity of advances and
innovation in materials used in medicine and
biotechnology, are testimony to the important scientific and
technological advances, which respond to the needs of human
beings caused mainly by the aging of the population and by
the appearance of bone diseases [1, 2]. One of the materials
studied to interact with biological systems is hydroxyapatite
(HAp), whose chemical formula is 



[3] and
presents a monoclinic structure with the space group P63/m
[3, 4]. It has been demonstrated, through experiments that the
HAp has bioactive, biocompatible, biostable and
osteoconductive characteristics [4-6]. In addition, it has
ventured into biomedicine as a restorative material, used in
ophthalmology, dentistry, and orthopedics [7-9]. In the latter,
favorable results have been found for bio-hydroxyapatite,
whose precursor is natural, and is present in bovine, porcine
and human bones, among others [4], [10, 11].
In the same way, the HAp is found in mineral rocks, and can
be obtained by synthesizing certain chemical components
[12], using methods such as: sol-gel, hydrothermal,
sonochemical, and the use of precursors from eggshells and
corals [13]. One of the main advantages of bio hydroxyapatite
is that it can be synthesized in large quantities from bio-waste
produced by cattle bones, which makes this source a more
ecological method in relation to others. However, some types
of synthesis may have disadvantages due to the absence of
osteoconductive and mechanical properties [14].
Within the synthesis processes of bio-hydroxyapatite are
degreasing, alkaline treatment and calcination [15].
Calcination is of particular importance because it eliminates
organic matter that has not been removed in other processes;
for this reason, analyzes have been made of the influence of
temperature on the structural, morphological and vibrational
properties of the HAp obtained from mammalian bones, where
an increase in the degree of crystallinity and crystal size has
been found with temperature, contrary to what occurs with
porosity. Likewise, it has been found with differential
calorimetric scanning and thermogravimetric analysis that for
T>700°C there are no organic components in the matrix and
that for T>800°C, an order-disorder transition occurs [16, 17].
Similarly, comparative studies of the quality of
biohydroxyapatite obtained from bovine bone with that of
commercial origin have been carried out [15], as well as the
growth of HAp crystals during the calcination process due to
the coalescence phenomenon for temperatures above 700°C,
and the way in which the Ca/P molar ratio decreases for
samples that are calcined at temperatures above 900°C [18].
Along the same lines, narrowing has been found in the X-ray
diffraction peaks due to crystalline growth at calcination
temperatures of approximately 700°C, confirming that
crystalline growth is a process that begins when the sample
has loss of organic matter and the change of bio-
hydroxyapatite from nano to microscale [19].
Consequently, the instrumental techniques and methods used
for the characterization of biomaterials and bone tissues are
vital for their study. These can be divided according to the
property to be studied, for example, crystallinity, particle size,
chemical and structural analysis, and morphology with
techniques in each of these classifications [20], all relevant to
make an analysis of the obtained HAp. Moreover,
thermogravimetric analysis and differential calorimetric
scanning provide important information on the properties and
transition phases when a sample is exposed to heating [21].
It is important to recognize the components of the natural
sources of HAp to identify what biomedical applications in
prosthesis or partial bone replacement could be made [22–24].
For this reason, some studies have analyzed the stability of
human bones and the extraction of type I collagen, finding that
the mineralization produces a change in the chemical and
mechanical properties of collagen in bone tissue, thereby
reducing its elasticity and resistance [8], [25].
In the bibliographic review few studies have been found with
ovine sources to produce hydroxyapatite [26, 27], in relation
to those of other animal sources. Therefore, the intention of
the article is to study the compositional, morphological, and
crystallographic properties of Hap obtained from sheep bones,
when varying the calcination temperature, and to analyze how
these modifications intervene in the Ca/P molar ratio. The
bone source was extracted from a slaughterhouse located in
Marulanda, Caldas, Colombia. This was intended to transmit
knowledge to the people of this community about the
preparation of this source of bio-HAp and to take advantage of
the organic waste from this place.
To carry out this study, the sheep femur bone powder was
synthesized from a male specimen approximately two years
old and characterized by means of thermogravimetric analysis
(TGA), scanning electron microscopy with elemental analysis
(SEM-EDS), X-ray diffraction (XRD) and Fourier transform
infrared spectroscopy (FTIR). It was found characteristic
peaks of HAp in the XRD analysis, and vibrational bands
inherent to the phosphate and hydroxyl functional groups with
FTIR.
This paper is structured as follows: first, the methodology
used for the synthesis of the ovine bones powder is described.
Then, the analysis of the characterization of the bone powder
samples is presented once they have been subjected to
different temperatures. Finally, the most relevant conclusions
of the study are reported.
II. METHODOLOGY
To carry out the synthesis of hydroxyapatite, the tibia and
femur bones of a male sheep of approximately 2 years were
used. Initially, the bone underwent a deproteinization phase,
which consists of carrying out a hydrothermal process, where
the bone marrow (diaphysis), patella, lipid membrane, and soft
tissues are first extracted. Subsequently, the bones are placed
in a pot with water, where they are cooked for approximately
30 minutes. Next, the tissues that could not be removed are
extracted and the bones are split into chips with a size of about
3 cm. Then, they are taken to a microwave oven at a power of
700W in a solution of water and detergent, for 30 minutes four
times, renewing the solution each time. Next, the bone chips
were washed with tap water, and later, the pieces were dried
I
Scientia et Technica Año XXVI, Vol. 26, No. 04, diciembre de 2021. Universidad Tecnológica de Pereira
527
by placing them in the microwave for 30 min without the
presence of liquid [5].
Then, the mechanical grinding of the bone pieces was carried
out. For this, a mill with stainless steel balls 304 was used at
100 rpm. They were ground for approximately two days at
intervals of time, until a powder of about 38 µm was obtained.
The samples were calcined in a muffle furnace Acequilabs
model MF-2003. The calcination temperatures of 600, 800 and
1000°C were used, with a ramp up of 5°C/min. N2 was used
as carrier gas, and once the desired temperature was reached,
the samples were left for 24 hours.
To characterize the samples, thermogravimetric analysis
techniques were used with a Q50 V20.13 Build 39 equipment,
at a ramp of 5°C/min from room temperature to 950°C. Also,
scanning electron microscopy with elemental analysis and X-
ray energy dispersion on a brand ZEISS Sigma 300
instrument. X-ray diffraction was performed on a D8 Bruker
AXS equipment with parallel beam geometry, using a Cu-Kα
source. Finally, Fast Fourier Transform Infrared Transmission
Spectroscopy (FTIR) with BRUKER equipment, platinum
Diamond 1 TTR accessory, and 4 cm-1 resolution was used.
Fig. 1 is a step-by-step summary of the synthesis and
characterization method of the obtained samples. In Fig. 2 (a)
the tibia and femur of the specimen are shown. Fig. 2 (b)
shows the pitcher used together with the heating rack and, in
Fig. 2 (c) the bone chips.
Fig 1. Block diagram for obtaining and studying HAp.
Fig 2. (a) sheep bones, (b) pressure cooker and, (c) bone chips.
III. RESULTS AND DISCUSSION
A. TGA and the first derivative
In Fig. 3, the thermogravimetric curve and the first derivative
of the TGA analysis of sheep bone powder sample can be
observed, showing the changes suffered when subjected to a
range from room temperature to 950°C. Thus, there is a
minimum mass loss between 400°C and 500°C (see Fig. 3(a)).
This denotes the decomposition of calcium hydroxide and
carbonates into water, and carbon dioxide [28].
Fig 3. (a) TGA sample curve of the sheep bones powder (b) first
derivative when samples are subjected to a range of temperatures from
room temperature to 950 °C with a rate of 5°C/min.
The changes produced at lower temperatures of around 670°C
correspond to the organic decomposition of fats and proteins
[17], [29], and for temperatures higher than this value the
thermal changes are related to the physicochemical
transformation of HAp [17].
The differences, due to the loss of mass between 200°C and
500°C correspond to the degradation and combustion of
collagen. When making the comparison between the TGA
curve with that of the first derivative (see Fig. 3 (b)), the
expected correspondence is found, with a peak that shows
considerable degradation at 644°C, due to the last protein
transformation.
According to TGA, a change of 9.67% occurs up to 200°C due
to the loss of water absorbed chemically and physically, and to
the decomposition of part of the organic matter. Therefore, a
difference of 32.04% is noted, and a considerable peak in the
curve of the first derivative, corresponding to the organic
decomposition and deneutralization of fats, which occurs
between 200 and 650°C, and a variation of 3.66% from 650°C
to 760°C due to the decomposition of the loss of carbonate
from the organic matrix and part of the carbonates. For
temperatures higher than 760°C and up to the limit of 950°C a
variation of 0.38%, which is normally due to the formation of
oxyapatite and oxide [17]. These last two percentages of
losses, when dealing with the decarboxylation of the sample,
gives way to the release of CO
2
.
Scientia et Technica Año XXVI, Vol. 26, No. 04, diciembre de 2021. Universidad Tecnológica de Pereira
528
B. Morphological Analysis
In order to evaluate the morphological changes of the sheep
bones powder when subjected to calcination processes, the
SEM technique was used. Fig. 4 (a) shows the sheep bones
powder without going through the calcination process, in
which the granulation process is not yet very evident. In Fig.s
4 (b) and 4 (c) samples, that were subjected to 600°C, 800°C
and 1000°C taken at 1000X are presented. According to the
TGA analyzes, mentioned above, the considerable loss of
mass up to 600 °C is not significant for the physical
transformations of the sample in Fig. 4 (a) with respect to 4
(b), this is because the thermal changes between these are
found associated with organic decomposition. Also, in both
are agglomerated grains forming cauliflower-like
distributions. On the other hand, in Fig.s 4 (c) and 4 (d), a
growth of the intergranular space can be observed, which can
be associated with the loss of the organic phase. The
morphology presents changes with the increase in temperature,
developing a spherical morphology. The formation of granules
increases and agglomeration in the samples decreases with
increasing temperature.
Fig 4. SEM photomicrographs (1000X). From (a) to (d) the uncalcined
sample, and those calcined at 600 °C, 800 °C and 1000 °C, respectively.
The X-ray energy dispersion spectrometry (EDX) technique
was used with the intention of finding the percentages of the
elements present in the studied samples. The results of the
chemical composition of the samples (uncalcined, 600 °C, 800
°C, and 1000 °C) show the presence of Ca, P, O and C, mainly
in the 600 °C. In the 800 °C samples the presence is less
which can be associated with the decarbonization process that
begins before 800 °C as is shown in the TGA measurements.
For the sample at 1000 °C, the presence of C is not seen
because at this temperature this process has already finished
Table I shows the Ca/P ratio for sheep bone powder samples
subjected to different temperatures. The sample without being
subjected to a calcination temperature shows a ratio of 2.22,
which may possibly indicate that there is a tetracalcium
phosphate at this point [30]. For the treatment at 600 °C it is
evidenced that the energy supplied, although it is sufficient to
promote the loss of organic matter, is not sufficient to achieve
the formation of stoichiometric hydroxyapatite. In addition,
the relationship is maintained in the apatite biological range.
TABLE I.
CA/P MOLAR RATIO OF THE SHEEP BONE POWDER (SBP) STUDIED SAMPLES.
Ca/P ratio
2.22
1.88
1.76
2.22
Now, for a sample subjected to 800 °C, the hydroxyapatite is
close to the stoichiometric type. At 1000 °C, the sample
becomes destabilized, causing an increase in the percentage of
calcium in relation to that of phosphorus, which indicates a
considerable substitution of phosphate ions for carbonate ions
[31]. Similarly, the calcium richness of the samples subjected
to 800 °C and 1000 °C can be associated with the CaO
impurity [32], which can be confirmed with the peaks of the
diffraction pattern.
C. X-Ray diffraction analysis
Fig. 5 represents typical patterns of HAp powder XRD,
synthesized at temperatures of 600°C, 800°C, and 1000°C,
respectively. They reveal the presence of HAp phases
consistent with the database found in Crystallography Open
Database with card 1521038 [33]. The main crystallographic
(hkl) planes for HAp: (002), (210), (211), (112), (022), (310),
(222) and (213) are identified in Fig. 3, showing as the most
intense the (211) plane. The percentages of crystallinity (1) of
the samples were 42.48, 89.94, and 89.77% for the samples at
600 °C, 800 °C and 1000 °C, respectively. This was calculated
using diffractograms, where the highest intensity peak and a
cautious near minimum were considered [34].




   (1)
Where
is the percentage of crystallinity,

is the highest
intensity peak (211), and

is the minimum intensity
between the previous plane and the (112) plane.
It is notorious that from 600 to 800 °C there is a considerable
increase in crystallinity, which is why at 600 °C the sample is
considered amorphous. At this temperature, the organic matter
has not been eliminated from the bone powder [5].
Scientia et Technica Año XXVI, Vol. 26, No. 04, diciembre de 2021. Universidad Tecnológica de Pereira
529
Fig 5. Diffraction patterns of the calcined samples at different
temperatures.
Additionally, the size of the crystallite associated with the
samples was found using the full width at half maximum
(FWHM), which is related to the Scherrer equation. The
crystallite sizes of 26.36 ± 7.80 nm, 54.42 ± 7.16 nm and
51.48 ± 5.47 nm were obtained for 600, 800 and 1000 °C,
respectively.
The changes in the mineral phase of bones due to the loss of
organic matter led to an increase in the size of the crystallite,
this is because the platelet habit of the bone mineral is lost
[35]. Thus, as the FWHM has been reduced, it is assumed that
the formation of hydroxyapatite crystals begins, giving way to
growth in crystallite sizes. At temperatures of 800 and 1000
°C it is found that there is stabilization of crystallite growth,
likewise, in the samples relative to these temperatures a peak
was found at 37.3° (2θ degrees) which is normally associated
with CaO and constitutes an undesirable impurity in Hap. This
is due to contact with water molecules, that results in breaking
and even some disintegration into individual particles and
alkalinity in the implant environment [32].
In addition, the lattice parameters of the hexagonal unit cell
were found a=b=9.39±0.06 Å and c=6.89±0.01 Å, which are
very close to those presented in the literature [19], [31], [36].
Moreover, it is observed that the size of the cell of the
structure is not affected by the change in temperature. This
stability can be associated with the presence of impurities such
as Mg, Na and

[5].
D. FT-IR analysis
In Fig. 6, it is possible to observe the infrared spectra of the
samples subjected to different temperatures. The vibration
bands corresponding to the characteristic functional groups for
hydroxyapatite such as phosphates 

and the hydroxyls

can be appreciated. However, the spectral lines also
show the presence of the carbonate group vibration

.These bands placed at 1415 and 875 

are associated with
symmetric n3 and asymmetric n2 stretching, respectively [36].
This corresponds to the substitution of

by 

in the
structure of HAp and it gives way to carbonate
hydroxyapatite. This substitution is typical in human bones,
promoting excellent biocompatibility and osteoconductivity
[37].
Fig 6. Infrared spectra of sheep bones powder without being subjected to
temperature and, subjected to 600, 800 and 1000 °C.
Additionally, the peaks close to 1620, 1320 and 782 

in
the green color graph (not subjected to calcination), can be
attributed to the presence of water and organic matter in the
sample before being subjected to temperature [38]. Likewise,
changes in the band close to 1000 

are associated with
the decrease in carbonates, which is related to the increase in
crystallinity [37]. It should be noted that the presence of
carbonate groups has origin in the natural source of obtaining
HAp.
IV. CONCLUSION
The results obtained show that the calcination temperature
influences the changes in the properties of the sheep bone
powder samples. With increasing temperature, forms closer to
stoichiometric hydroxyapatite, higher degrees of crystallinity,
and larger crystallite sizes are found. Also, for temperatures of
600 °C, a total loss of water and organic matter from the
sample is observed. There is loss of carbonates at higher
temperatures. This is evident in the FT-IR spectra, which
added to the TGA results leads to suggest that 760 °C is an
Scientia et Technica Año XXVI, Vol. 26, No. 04, diciembre de 2021. Universidad Tecnológica de Pereira
530
appropiated temperature to obtain protein-free samples. In
addition, the presence of CaO was detected in the
diffractograms, which confirms that the samples obtained at
800 °C and 1000 °C are rich in Ca. The samples Ca/P ratio is
higher than pure HAp, being the closest relation to this the 800
°C sample with a value of 1.76. Likewise, the reduction in the
FWHM of the peaks in XRD represents an increase in the
formation of crystals and in their size. It is found that this
occurs as the calcination temperature increases as shown in the
samples of SEM. This increment rises the formation of grains
due to the phenomenon of coalescence, i.e., this temperature
supplies energy for the formation of the crystallites. It should
be noted that the increase in the FWHM is not necessarily
linked to the quality of the crystallites. However, the lattice
parameters of the crystal structure do not present major
variations with temperature, it is feasible to associate it with
the presence of impurities such as carbonates because the
study material comes from a biogenic source. On the other
hand, it should be noted that there is a need of samples
calcination when they come from animal sources. As was
mentioned earlier, at temperatures below 600 °C the sample is
considered amorphous. For future studies, it is recommended
to take temperature values between 600 and 800 °C, and 800
and 1000 °C, since for the Ca/P ratio considerable changes
occur between these temperature range. Finally, according to
the obtained results, the samples calcined at 800 °C are
considered promising for biocompatibility studies.
REFERENCES
[1] Hardouin, P. Les biomatériaux de l’appareil locomoteur. Rev Rhum
Mal Ostéoartic 1992, volume 59, page range: 829-833.
[2] Ratner, B.D; Hoffman, A.S; Schoen, F.J; Lemons, J.E. Biomaterials
science: an introduction to materials in medicine, 3rd ed.; California,
San Diego, 2004; pp. 157-196.
[3] Aquilano, D; Bruno, M; Rubbo, M; Massaro, F.R; and Pastero, L. Low
symmetry polymorph of hydroxyapatite. theoretical equilibrium
morphology of the monoclinic Ca5(OH)(PO4)3. Cryst. Growth Des.
2014, volume 14, page range: 2846–2852.
[4] Garcia-Garduño, M.V.; Reyes-Gasga, J. La hidroxiapatipa, su
Importancia en los Tejidos Mineralizados y su aplicación. Rev. Espec.
en Ciencias Químico-Biológicas 2006, volume 9(2), page range: 90-95.
[5] Forero, P.A. Influencia de la Temperatura en Hidroxiapatita Extraida a
Partir de Hueso de Cerdo.Tesis de maestria, Universidad Nacional de
Colombia, Manizales,2017.
[6] Alghamdi, M.M.; Awwad, N.S.; Al-Sharaey, A.A., Abd-Rabboh, H. S.,
and Keshk, S. M. Physicochemical characterization of natural
hydroxyapatite/ cellulose composite. Indian Journal of Fibre and
Textile Research 2019, volume 44 (1), page 45-50.
[7] Janus, A. M.; Faryna, M.; Haberko, K.; Rakowska, A.; Panz, T.
Chemical and microstructural characterization of natural
hydroxyapatite derived from pig bones. Microchim 2008, volume 161,
page range: 349-353.
[8] Lozano, L.F.; Peña-Rico, M.A.; Heredia, A. et al. Thermal analysis
study of human bone. Journal of Materials Science 2003, volume 38,
page range: 4777–4782.
[9] Raya, I.; Mayasari, E.; Yahya, A.; Syahrul, M.; Latunra, A. I.
Shynthesis and Characterizations of Calcium Hydroxyapatite Derived
from Crabs Shells (Portunus pelagicus) and Its Potency in Safeguard
against to Dental Demineralizations. Int. J. Biomater 2015, volume
2015, page range: 1–8.
[10] Boutinguiza, M.; Pou, J.; Comesaña, R.; Lusquiños, F.; de Carlos, A.;
León, B. Biological hydroxyapatite obtained from fish bones. Mater.
Sci. Eng. C 2018, volume 32, page range: 478-486.
[11] González-Rodríguez, L.; López-Álvarez, M.; Astray, S.; Solla, E. L.;
Serra, J.; González, P. Hydroxyapatite scaffolds derived from deer
antler: Structure dependence on processing temperatura. Mater. Charact
2019, volumen 155, page range: 1-13.
[12] Buddy, D.; Ratner, A.S.; Hoffman, F. J.; Schoen, J.E. An introduction
to materials in Medicine, 3rd ed.; California, San Diego, 1996; pp. 289-
352.
[13] Sadat-Shojai, M.; Khorasani, M.T.; Dinpanah-Khoshdargi, E.;Jamshidi,
A. Synthesis methods for nanosized hydroxyapatite in diverse
structures. Acta Biomater 2013, volume 2013, page range: 31.
[14] Figueiredo, M.; Fernando, A.; Martins, G.; Freitas, J.; Judas, F.;
Figueiredo, H. Effect of the calcination temperature on the composition
and microstructure of hydroxyapatite derived from human and animal
bone. Ceram. Int 2010, volume 36, page range: 2383-2393.
[15] Rodriguez-García, M. E.; et al. Comparison of physicochemical
properties of bio and commercial hydroxyapatite. Curr. Appl. Phys
2013, volume 13, page range: 1383-1390.
[16] Taubert, A.; et al. Water-soluble cellulose derivatives are sustainable
additives for biomimetic calcium phosphate mineralization. Inorganics
2016, volume 4, page range:1-17.
[17] Ramirez-Gutierrez, C. F.; Londoño-Restrepo, S. M.; del Real, A.;
Mondragón, M. A.; Rodriguez-García, M. E. Effect of the temperature
and sintering time on the thermal, structural, morphological, and
vibrational properties of hydroxyapatite derived from pig bone.
Ceramics International 2017, volume 43, page range: 7552-7559.
[18] Londoño-Restrepo, S. M.; Jeronimo-Cruz, R.; Rubio-Rosas, E.;
Rodriguez-García, M. E. The effect of cyclic heat treatment on the
physicochemical properties of bio hydroxyapatite from bovine bone. J.
Mater. Sci. Mater. Med 2018, volume 2018, page range: 29–52.
[19] Londoño-Restrepo, S. M.; Millán-Malo, B. M.; del Real-López, A.;
Rodriguez-García, M. E. In situ study of hydroxyapatite from cattle
during a controlled calcination process using HT-XRD. Mater. Sci.
Eng. C 2019, volume 105, page range: 110020.
[20] Miti, Z.; et al. Instrumental methods and techniques for structural and
physicochemical characterization of biomaterials and bone tissue: A
review. Mater. Sci. Eng. C 2017, volume 79, page range: 930-949.
[21] Ellingham, S. T. D.; Thompson, T. J. U.; Islam, M. Thermogravimetric
analysis of property changes and weight loss in incinerated bone.
Palaeogeogr. Palaeoclimatol. Palaeoecol 2015, volume 438, page
range: 239-244.
[22] Stevens, M.M. Biomaterials for bone tissue engineering (Review).
Mater today 2008, volume 11, page range: 18-25.
[23] Krishna, D. S. R.; Chaitanya, C. K.; Seshadri, S. K.; Kumar, T. S. S.
Fluorinated hydroxyapatite by hydrolysis under microwave irradiation.
Trends Biomater, Artif. Organs 2002, volume 16, page range: 15-17.
[24] Rajendran, J.; Gialanella, S.; Aswath, P.B. XANES analysis of dried
and calcined bones. Mater. Sci. Eng. C 2013, volume 33, page range:
3968–3979.
[25] Schumacher, T.C.; et al. A novel, hydroxyapatite-based screw-like
device for anterior cruciate ligament (ACL) reconstructions. Knee
2017, volume 24, page range: 933-939.
[26] Akyurt, N.; Yetmez, M.; Karacayli, U.; Gunduz, O. A New Natural
Biomaterial: Sheep Dentine Derived Hydroxyapatite. Key Eng. Mater
2012, volume 494, page range: 281-286.
[27] Duta, L.; et al. Comparative physical, chemical and biological
assessment of simple and titanium-doped ovine dentine-derived
hydroxyapatite coatings fabricated by pulsed laser deposition. Appl.
Surf. Sci 2017, volume 413, page range: 129-139.
[28] Poovendran, K.; Joseph-Wilson, K. S. Amalgamation and
characterization of porous hydroxyapatite bio ceramics at two various
temperatures. Mater. Sci. Semicond. Process 2019, volume 100, page
range: 255–261.
[29] Ramirez-gutierrez, C. F.; London, S. M.; Rubio-Rosas.; Study of
bovine hydroxyapatite obtained by calcination at low heating rates and
cooled in furnace air. Mater. Sci 2016, volume 51, page range: 4431-
4441.
[30] Bohner, M. “Calcium orthophosphates in medicine: from ceramics to
calcium phosphate cements,” Int. J. Care Inj., 2000.
[31] Kumar, S.; Jahan, R. A.; Yee, S.; Li, X.; and Arafat, M. T. “Effects of
organic modifiers and temperature on the synthesis of biomimetic
carbonated hydroxyapatite,” vol. 45, no. May, pp. 24717–24726, 2019.
[32] Sobczak-kupiec, A. and Wzorek Z. “The influence of calcination
parameters on free calcium oxide content in natural hydroxyapatite,”
Ceram. Int., vol. 38, no. 1, pp. 641–647, 2012.
[33] Fleet, M. E.; Liu, X.-Y. and Pan, Y.-M. “Site preference of rare earth
elements in hydroxyapatite Ca10 (P O4)6 (O H)2,” J. Solid State
Chem., vol. 149, pp. 391–398, 2000.
[34] Alshemary, Z.; Akram, M.; Goh, Y. F.; Abdul Kadir, M. R.; Abdolahi,
A. and Hussain, R. “Structural characterization, optical properties and
Scientia et Technica Año XXVI, Vol. 26, No. 04, diciembre de 2021. Universidad Tecnológica de Pereira
531
in vitro bioactivity of mesoporous erbium-doped hydroxyapatite,” J.
Alloys Compd., vol. 645, pp. 478–486, 2015.
[35] Mucalo, M. R. Animal-bone derived hydroxyapatite in biomedical
applications. Elsevier Ltd., 2015.
[36] León, B. and Jansen, J. A. Thin Calcium Phosphate Coathings for
Medical Implants, Springer S. 2009.
[37] Bartnicka, S.; Borkowski, L.; Ginalska, G.; Ślósarczyk, A. and
Kazarian, S. G. “Structural transformation of synthetic hydroxyapatite
under simulated in vivo conditions studied with ATR-FTIR
spectroscopic imaging,” Spectrochim. Acta - Part A Mol. Biomol.
Spectrosc., vol. 171, pp. 155–161, 2017.
[38] Londoño-Restrepo, S. M.; Zubieta-Otero, L. F.; Jeronimo-Cruz, R.;
Mondragon, M. A. and. Rodriguez-García, M. E .“Effect of the crystal
size on the infrared and Raman spectra of bio hydroxyapatite of human,
bovine, and porcine bones,” J. Raman Spectrosc., vol. 50, no. 8, pp.
1120–1129, 2019.
Valentina Restrepo-Ramírez was born in
Pereira, Risaralda, Colombia in 1997. She
graduated from engineering physics
program at Technological University of
Pereira (UTP), Risaralda, in 2020. She has
worked in different research groups at
UTP. Her research interest is related to the
development of novel materials, in special,
biomaterials for medical goals. Ms. Restrepo has been
member of SPIE (The International Society for optics and
photonics), OSA (The Optical Society) and Colombian
Society of Physics Engineering.
ORCID: https://orcid.org/0000-0001-6093-5594
Iván Darío Arellano-Ramírez was
born in Pereira, Colombia. He received
the B.S. degree in physical engineering
from Peter the Great St. Petersburg
Polytechnic University, Russia, in 2006
and the M.S. degree in applied physics
from Gwangju Institute of Science and
Technology, South Korea, in 2009. He
is currently pursuing a Ph.D. degree in physics at the National
University of Colombia, Manizales, Colombia.
From 2007 to 2009 he was a Research Assistant at the Xray
Laboratory for Nanoscale Phenomena, Gwangju Institute
of Science and Technology, South Korea. Since 2010, he has
been a Professor with the Department of Physics at
Technological University of Pereira. His research interests
include simulation of photovoltaic cell technology, quantum
dots, materials characterization techniques. Since 2019 he is
member of SPIE and OSA.
ORCID: https://orcid.org/0000-0002-6337-7644
Natalia Alzate-Acevedo
She received the B.S. degree n physical
engineering in 2018. She is currently
pursuing a M. S degree in physical
science at National University of
Colombia, Manizales. She has 7 years
of experience in synthesis and
characterization of nanostructured
materials. She has participated in
scientific events and academic projects.
ORCID: https://orcid.org/0000-0002-7557-6771
Elisabeth Restrepo-Parra
She is an electrical engineer, M.S. in
physical science and PhD in engineering.
She has research experience of more than
20 years in simulation of bulk materials,
nanoparticles and multilayers by stochastic
methods (Molecular Dynamics and Monte Carlo) for the
evaluation of magnetic, mechanical and ferroelectric
properties. Additionally, she has worked on synthesis,
production and characterization of PAVD-assisted coatings,
manganites by hydrothermal route and different methods of
obtaining nanostructures.
She has published more than 250 scientific papers, published
in high-impact journals. In addition, she has published one
book and 6 book chapters. In her academic experience, she has
conducted undergraduate and graduate subjects such as Solid
State Physica, Modern Physics, Gas Discharges, among
others. She has supervised more than 70 undergraduate and
graduate theses.
ORCID: https://orcid.org/0000-0002-1734-1173
Carlos Daniel Acosta-Medina
He received a B.S. degree in Mathematics
from the University of Sucre, Colombia, a
M.S. in mathematics and a PhD in
mathematics from the National University of
Colombia, Medellín. He also has a
postdoctoral stay in Mathematical Engineering at the
University of Concepción. He has more than 20 years in
educational experience and is Professor in the area of
mathematics at the National University of Colombia,
Manizales since 2000. He has held academic administrative
positions as director of research and extension at UNAL-
Manizales and, currently dean of the Faculty of Natural
Sciences of this Institution. In addition to this, he participates
in the development of research and extension activities, and
projects focused on the approach of the University with the
basic secondary institutions.
ORCID: https://orcid.org/0000-0002-6477-8984