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Synthesis and characterization of pure and nanosized hydroxyapatite bioceramics

  • Aneela Anwar

    Aneela Anwar completed her PhD from University College London, UK, on Islamic Development Bank Merit Scholarship. She returned to her organization, University of Engineering and Technology and has been chairing the basic sciences department. She has presented her quality research work at various national and international podia. The nature of her work, supreme presentation skills and innovation ideas had been appreciated much. She holds a patent besides various research publications. Her research mainly deals with the investigation of novel synthesis methodologies and analysis of various high purity nanoscale biomedical materials as medical device for hospitals/orthopaedic surgeon and research field.

     ORCID logo EMAIL logo     , Qudsia Kanwal

    Qudsia Kanwal received her PhD degree from University of Punjab Pakistan as an HEC scholar. She worked as an assistant professor in Lahore College for women university Lahore and as visiting Faculty in University of Engineering and Technology, Lahore. Now she is working as an assistant professor in the University of Lahore. Her research interests are biopesticides synthesis, green chemistry and nanochemistry.

         , Samina Akbar

    Samina Akbar is an Assistant Professor of Chemistry at the University of Engineering and Technology Lahore, KSK campus, Pakistan. Her research interests embrace the use of Lyotropic Liquid Crystals as a template for the production of highly ordered nanostructured platinum materials. She is investigating the fabrication and characterization of nanostructured materials. These materials exhibit very high surface area, high conductivity, and chemical stability which make them ideal for use in the next generation energy storage and energy conversion devices.

         , Aisha Munawar

    Aisha Munawar completed her Masters (1998) and MPhil studies in inorganic Analytical chemistry from the Quaide-Azam University in 2000. She joined the Department of Chemistry, University of Engineering and Technology, Lahore, in 1999 as a lecturer. Later she completed her doctorate studies at The University of Hamburg, in 2012. Her research interests are proteomics, peptide isolation and characterization, snake venom, inorganic chemistry and biomaterials.

         , Arjumand Durrani

    Arjumand Iqbal Durrani did her MSc and MPhil in chemistry from the University of Engineering and Technology, Lahore and University of Punjab, Lahore, respectively. She has done PhD from University of Vienna, Austria, in the field of analytical and food chemistry. She has research interest in the field of analytical chemistry, food chemistry, nanotechnology and environmental chemistry. She has more than 12 years of teaching experience both at graduate and post-graduate level.

         and Masood Hassan Farooq

    Masood Hassan Farooq is working as an Assistant Professor of Physics in the University of Engineering and Technology, Lahore since September 2015. He has joined the Laboratory of Eco-Materials and Sustainable Energy Post-Doct research of The Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Urumqi, P. R. China (2013–2015). He worked on the fabrication of advanced functional materials and their environmental applications. He got the doctorate degree in Applied Physics from the University of Science and Technology Beijing (USTB), P. R. China (2010–2013). He has published 23 scientific articles in different journals, i.e. Crystal Engineering Communication, RSC Advance, Material Letters having IF above 45.
Published/Copyright: July 12, 2016
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Nanotechnology Reviews
From the journal Nanotechnology Reviews Volume 6 Issue 2

Abstract

Synthetic nanosized hydroxyapatite (HA) particles (<120 nm) were prepared using a co-precipitation technique by adopting two different routes – one from an aqueous solution of calcium nitrate tetrahydrate and diammonium hydrogen phosphate at pH 10 and the other by using calcium hydroxide and phosphoric acid as precursors at pH 8.5 and reaction temperature of 50°C. The lattice parameters of HA nanopowder were analogous to reference [Joint Committee on Powdered Diffraction Standards (JCPDS)] pattern no. 09-432. No decomposition of HA into other phases was observed even after heating at 1000°C in air for 1 h. This observation revealed the high-temperature stability of the HA nanopowder obtained using co-precipitation route. The effects of preliminary Ca/P molar ratio, precipitation, pH and temperature on the evolution of phase and crystallinity of the nanopowder were systematically examined and optimized. The product was evaluated by techniques such as X-ray-diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) and Raman spectroscopy analyses. The chemical structural analysis of the as-prepared HA sample was performed using X-ray photoelectron spectroscopy (XPS). After heat treatment at 1000°C for 1 h and ageing for 15 h, the product was obtained as a phase-pure, highly crystalline HA nanorods.

Keywords: bioceramics; hydroxyapatite (HA); nanorods; X-ray diffraction

1 Introduction

Ca10(PO4)6(OH)2 (hydroxyapatite, HA) is the key mineral constituent of bone and teeth [1] and has attracted much attention in orthopaedics and plastic surgery in recent years because of its biocompatibility, bioactivity and low solubility in wet media [2]. Hence synthetic nano-HA powder is of abundant interest as a bone replacement and strengthening material in biomedical composites. Such nanobioceramics have been utilized as a scaffold material to encourage new bone growth for osteographical coatings on metal implants [3], [4], [5], [6], [7]. Many techniques have been described in literature for the synthesis of HA including solid-state synthesis [8], sol gel techniques [8], [9], [10], spray pyrolysis [11], solvothermal processes [12] and chemical vapour deposition [13]. Among others wet chemical precipitation technique was employed for the batch synthesis of phase-pure HA nanopowder from aqueous solution of diammonium hydrogen phosphate, calcium nitrate and ammonium hydroxide, respectively [14].

Two precipitation methods have been reported in literature [15], [16] for HA production. In the first method the reaction was carried out by mixing 0.6 m phosphoric acid solution with 1 m calcium hydroxide solution.

10 [Ca (OH)2]+6H3PO4→[Ca10(PO4)6(OH)2]+18 H2O

The second coprecipitation method was based on the addition of diammonium hydrogen phosphate into the solution of calcium nitrate and ammonium solution as agent for pH adjustment (method we have adopted for HA synthesis). Similar work has been done by Liu et al. [17]. They described the mechanism and kinetic studies of HA precipitation at pH 10–11 which were greatly affected by variation in time and Ca:P ratio under different temperatures. The properties and nature of the synthesized HA powder depended mainly on the temperature, pH, time and other precipitation conditions like ageing time, variation in Ca:P ratio [18], [19], [20]

6[(NH4)2HPO4]+10[(Ca(NO3)2.4H2O] +8NH4OH→20 NH4NO3+[Ca10(PO4)6(OH)2] +46 H2O

In this article, we describe about the experimental studies where we have controlled synthesis for stoichiometric HAs with 1.67 Ca/P ratio using calcium ion and phosphate ion source as starting materials by adding ammonium hydroxide at 50°C. The main aim of this study is to synthesise phase-pure nanosized HA powder for bone replacement applications using co-precipitation technique at low temperature and relatively lesser time period with improved yield and smaller particle size compared to conventional literature methods.

2 Materials and methods

2.1 Reagents and materials

Calcium hydroxide [98%], diammonium hydrogen phosphate [98%], calcium nitrate tetrahydrate [99%], and phosphoric acid [97%] were purchased from Alpha Aesar Chemical Company (Dorset, UK). Ammonium hydroxide solution [NH4OH (aq.), 28 vol%] was supplied by VWR International (East Grinstead, UK). Deionised (DI) water was used in all experiments.

2.2 Experimental

2.2.1 Synthesis of stoichiometric nano-hydroxyapatite

2.2.1.1 Method 1

The phase-pure nano-HA was prepared using a co-precipitation method. The reagents used in the process were 0.15 m diammonium hydrogen phosphate solution and 0.25 m calcium nitrate solution, respectively (Ca:P=1.67). The pH of the precursors was made up to 10 by adding 5.0 and 10.0 ml of ammonium hydroxide to calcium nitrate and diammonium hydrogen phosphate solutions, respectively, with constant mechanical stirring. In this method, 250 ml PO43- ion solution was added dropwise to 250 ml Ca2+ ion solution with the flow rate of 10 ml/min in order to yield an amorphous precipitate of HA at a reaction temperature of 50°C. The pH of the suspension was monitored regularly throughout the addition. Reactions carried out in basic conditions resulted in the formation of stoichiometric HA. The aqueous suspension was first aged for 15 h and then dispersed in 45 ml DI water using a vortex mixer followed by three further washing cycles. The wet residue was then oven dried at 90°C for 12 h prior to further analysis.

2.2.1.2 Method 2

In the second process, HA samples were prepared by wet precipitation by addition of orthophosphoric acid (0.15 m) to calcium hydroxide (0.25 m) slurry. The samples were synthesized with 1.67 Ca:P ratio at pH 8.5 with constant mechanical stirring at 50°C. The pH of the suspension was monitored regularly throughout the addition. The aqueous suspension collected from this procedure was aged for 15 h, washed (three times), centrifuged and then oven dried as mentioned earlier.

Each of the as-prepared HA samples was heat treated at 1000°C for 1 h in air at a heating rate of 10°C/min as per ISO standard methods [ISO13779-3] to confirm the thermal stability and phase purity of the obtained nanopowder. The dried product was free flowing fine white powder with ~89% yield.

2.3 Characterization methods

2.3.1 Transmission electron microscopy

The TEM images were obtained using a JEOL JEM-1200EX II electron microscope. A small amount of sample (<10 mg) was dispersed in neat methanol and then ultrasonicated for 2 min to yield a very dilute suspension. A few drops of the resulting suspension were then deposited on a carbon-coated copper grid, which was used as the TEM specimen. The grid was dried prior to use in the double-tilt holder of the TEM. Image J software (version 5.0) was used to estimate the particle size.

2.3.2 Powder X-ray diffraction

Bruker AXS D4 Endeavour™ XRD diffractometer was used for XRD collection of all samples. The data were collected from 20 to 40° in 2θ range with 0.04° scanning step and a count time of 2 s using Cu-Kα radiation (λ=1.5406 Å). DIFFRACplus Eva™ software was used for the phase analysis of the data by spectral matching with standard patterns. The crystallite sizes were calculated by using the Debye-Sherrer equation [21].

2.3.3 Dynamic light scattering

Dynamic light scattering (DLS) measurements were performed using a Malvern Instruments Zetasizer operated in backscatter (173°) mode. The sample slurry was produced with a solid content ~1% by volume and diluted with methanol. To disperse the sample, this suspension was kept in an ultrasonic bath for 10 min. Square cuvettes with a path length of nominally 10 mm were used for measurements.

2.3.4 Fourier transform infrared spectroscopy

The functional groups on HA surface were interrogated using FTIR – a Nicolet 6700 FTIR. The FTIR spectra were obtained between 400 and 4000 cm-1 range at a resolution of 4 cm-1 averaging 256 scans.

2.3.5 Raman spectroscopy

A confocal Raman DXR spectrometer (SP Thermo-Scientific) was used. The powder sample was deposited onto 316 L stainless steel block using a spatula. First, the 316 L block was wiped clean using distilled water and then with acetone prior to sample analysis. The data were collected using 780 nm laser, 10 X Lens with the scan time of 90 s for each sample.

2.3.6 Chemical analysis

Chemical analysis of HA samples was carried out using a thermo scientific K-alpha X-ray photoelectron spectrometer with a two-chamber vacuum system. The spectrum was collected at 50 eV for high resolution areas and for survey scans at 150 eV. The sensitive detector, a 128-channel position was used. The XPS spectra were processed using Casa™ software. A C 1 s peak at 285.0 eV calibrated the binding energy scale.

3 Results and discussion

3.1 Transmission electron microscopy

The TEM images of the samples obtained from reactions 1 and 2 as shown in Figure 2 confirmed that small crystallites had been formed. Phase-pure HA nanoparticles synthesized using co-precipitation method 1, had a rod-like morphology and an average length along the longest axis of each particle was ~115±15 and ~15±5 nm (200 particles sampled) along the smaller axis (Figure 1A, B). The SEM images were also captured for both as-prepared and heat-treated (1000°C, 1 h) nano-HA samples as mentioned in Figure 2A, B, respectively.

Figure 1: TEM images of as-prepared phase-pure hydroxyapatite nanorods prepared by using method 1 based on calcium nitrate and diammonium hydrogen phosphate precursors (A) bar=200 nm, and (B) bar=100 nm, via co-precipitation method.
Figure 1:

TEM images of as-prepared phase-pure hydroxyapatite nanorods prepared by using method 1 based on calcium nitrate and diammonium hydrogen phosphate precursors (A) bar=200 nm, and (B) bar=100 nm, via co-precipitation method.

Figure 2: SEM images of as-prepared (A) and heat-treated (B) phase-pure hydroxyapatite nanorods prepared by using method 1 based on calcium nitrate and diammonium hydrogen phosphate precursors with bar size 100 nm.
Figure 2:

SEM images of as-prepared (A) and heat-treated (B) phase-pure hydroxyapatite nanorods prepared by using method 1 based on calcium nitrate and diammonium hydrogen phosphate precursors with bar size 100 nm.

3.2 Dynamic light scattering

Particle size distribution was also conducted for as-prepared HA samples prepared using methods 1 and 2, respectively. The DLS measurements of pure HA sample 1 reveal an average particle size of ca. 158 nm and a polydispersity index (PDI) value of 0.231. Whilst for sample 2, DLS measurements yielded an average particle size of ca. 160 nm and a PDI value of 0.268 with unimodal distribution of particles.

The DLS measured diameter between 100 and 300 nm with a PDI value of 0.3 or less displays good dispersion results. It was also seen that DLS measurement results are in good agreement with TEM-determined distributions as shown in Table 1.

Table 1:

Lattice parameters, crystalline size, particle size and hydrodynamic diameter of nanosized hydroxyapatite particles.

Sample IDXRD lattice parametersXRD crystallite size (nm)TEM crystallite size (nm)DLS hydrodynamic diameter (nm)
a (Å)c (Å)
HA-19.42±0.00236.89±0.0122112115158
HA-29.42±0.00256.88±0.0124108110160

3.3 X-ray diffraction analysis

The X-ray diffraction data of phase-pure HAs displayed broad peak of an apatite structure (Figure 3). Upon heat treatment (1000°C for 1 h), the X-ray diffraction peaks became considerably sharper and well resolved and gave an excellent match to the phase-pure HA reference (JCPDS) pattern no. 09-432. No additional peaks of beta-tricalcium phosphate (TCP) were observed in the XRD data even after heat treatment at 1000°C, which would have suggested secondary phases as shown in Figure 4. Thus, the results indicated the phase purity and high-temperature stability of the obtained nano-HA product. The XRD lattice parameters a and c obtained from this report are correlated with the literature findings [22] for the stoichiometric HA (JCPDS [-09-432], a=9.41 Å and c=6.88 Å) as shown in Table 1.

Figure 3: X-ray powder diffraction patterns of phase-pure, as-prepared hydroxyapatite nanorods synthesized using method 1 (A) and method 2 (B) via co-precipitation technique.
Figure 3:

X-ray powder diffraction patterns of phase-pure, as-prepared hydroxyapatite nanorods synthesized using method 1 (A) and method 2 (B) via co-precipitation technique.

Figure 4: Powder X-ray diffraction patterns of heat-treated, phase-pure hydroxyapatite nanorods, synthesized using method 1 (A) and method 2 (B) via co-precipitation technique.
Figure 4:

Powder X-ray diffraction patterns of heat-treated, phase-pure hydroxyapatite nanorods, synthesized using method 1 (A) and method 2 (B) via co-precipitation technique.

3.4 Fourier transform infrared spectroscopy

Raman and FTIR spectroscopies were utilized to analyse the samples and aid in the identification of different calcium phosphates. The FTIR data of as-prepared HA samples showed bands at 3420 cm-1 stretching mode (νs) corresponding to stretching vibrations of the hydroxyl group in HA [6]. The bands at 1637 cm-1 revealed the bending mode for lattice water as shown in Figure 5. The FTIR band at 1453 cm-1 was characterized to the stretching mode (ν3) of some adsorbed carbonate ions on HA surface. The band at 1031 cm-1 displayed the phosphate asymmetric stretching mode (ν1), whereas the O-P-O bending modes were assigned to 632 and 534 cm-1 (ν4) respectively.

Figure 5: FTIR spectra of phase-pure hydroxyapatite nanorods, prepared by using method 1 (A) and method 2 (B) via co-precipitation technique.
Figure 5:

FTIR spectra of phase-pure hydroxyapatite nanorods, prepared by using method 1 (A) and method 2 (B) via co-precipitation technique.

3.5 Raman spectroscopy

Raman spectroscopy was carried out in order to supplement the crystallographic data and detect substitutions in the apatite lattice. The band at 965 cm-1 attributed to a symmetric stretching of P-O bond in phosphate [23], [24]. The bands at 610, 593 and 583 cm-1 are corresponded likely to the O-P-O linkage bending mode in phosphate. Whilst the peaks at 1078, 1049 and 1030 cm-1 revealed the asymmetric stretching of P-O bond in phosphate as shown in Figure 6.

Figure 6: Raman spectra of phase-pure hydroxyapatite nanorods of sample 1, synthesized by using diammonium hydrogen phosphate and calcium nitrate precursors (A) and sample 2, synthesized using calcium hydroxide and orthophosphoric acid precursors (B) via co-precipitation method.
Figure 6:

Raman spectra of phase-pure hydroxyapatite nanorods of sample 1, synthesized by using diammonium hydrogen phosphate and calcium nitrate precursors (A) and sample 2, synthesized using calcium hydroxide and orthophosphoric acid precursors (B) via co-precipitation method.

Bands at 610, 593 and 583 cm-1 are corresponded likely to the bending mode (ν4) of the O-P-O linkage in phosphate. Whilst the bands at 1078, 1049 and 1030 cm-1 assigned to asymmetric stretching (ν1) of the P-O bond in phosphate as shown in Figure 6.

3.6 Chemical analysis

A chemical analysis of the as-prepared HA sample using co-precipitation was done by using XPS analysis as shown in Figure 7. The peaks at 134 eV corresponded to P 2p spectra of HA. While the binding energy values for O 1s and Ca 2p were measured as 532 and 347 eV, respectively. The Ca/P ratio in the analysed samples was close to the stoichiometric ratio of 1.67 as shown in Table 2.

Figure 7: XPS survey spectrum of phase-pure hydroxyapatite nanorods of sample 1, synthesized using calcium nitrate and diammonium hydrogen phosphate precursors via co-precipitation method.
Figure 7:

XPS survey spectrum of phase-pure hydroxyapatite nanorods of sample 1, synthesized using calcium nitrate and diammonium hydrogen phosphate precursors via co-precipitation method.

Table 2:

Quantitative analysis of as-prepared hydroxyapatite samples by using X-ray photoelectron spectroscopy: relative chemical compositions (atomic %).

Sample nameC 1sO 1sCa 2pP 2pCa/P
HA-1 (using method 1)26.6747.0216.439.881.66
HA-2 (using method 2)26.7847.7515.859.621.65

The individual spectra for Ca, O and P for HA sample prepared using method 1 is presented in Figure 8. The resolution of Ca 2p spectrum into two peaks 2p1/2 and 2p3/2 at 351.3 and 347.4 eV, respectively, are related to HA. In Figure 8B, the 2p peak can also be deconvoluted into two peaks with a spin orbit splitting for p1/2 and p3/2 levels with binding energies 134.2 and 133.4 eV, respectively [25], [26], [27].

Figure 8: XPS spectra of (A) Ca 2p, (B) P 2p and (C) O 1s for phase-pure hydroxyapatite nanorods of sample 1, synthesized with the help calcium nitrate and diammonium hydrogen phosphate precursors via co-precipitation method.
Figure 8:

XPS spectra of (A) Ca 2p, (B) P 2p and (C) O 1s for phase-pure hydroxyapatite nanorods of sample 1, synthesized with the help calcium nitrate and diammonium hydrogen phosphate precursors via co-precipitation method.

Figure 8C depicts the core level XPS spectrum of O 1s, the peaks at 532.1 and 531.5 eV are assigned to the hydroxyl group and contribution of phosphate group, respectively.

In this research, it was observed that the particle properties could be affected, e.g. such as particle size and shape, by selection of conditions such as the temperature, reaction pH and variation in Ca:P ratio. A careful control of reaction conditions is very important in order to get the phase-pure product. Most of the room temperature co-precipitation syntheses require longer reaction time with extensive stirring and ageing from 24 h to a couple of weeks in order to achieve a phase-pure product [28], [29]. In this study, a slight variation in the reaction temperature from room temperature to 50°C, reduced ageing time considerably from 24 h to 15 h along with an enhanced product yield. The reason for using high-temperature strategy for this particular study was to speed up the reaction kinetics and precursor’s dissolution rate in order to achieve maximum yield in relatively shorter time period [30]. As a consequence, the reaction time decreased with significant increase in the reaction yield. This study confirmed that the reaction time and temperature are two important factors in order to evaluate the phase purity, crystallite size and product yield. We also investigated that by lowering the reaction temperature, small particle size (<100 nm) of nano-HA could be achieved but this would increase the ageing time from 15 h to 24 h. Thus, by modifying reaction parameters such as temperature, time, etc., any suitable nanoproduct with required particle size could be obtained by exploiting the recent studies. This would mean that these nanobioceramics could be acceptable for clinical use according to the latest international standards and guidelines.

Thus the process represents a low cost, synthesis technique, which works near ambient temperature and atmospheric pressure and allows the synthesis of high-purity stoichiometric HA and other bioceramic materials in lesser time period compared to traditional literature findings (which required 24 h or more) with fine control over the particle size.

4 Conclusions

In summary, co-precipitation technique provides a facile and economical pathway to obtain nanosized HA and other calcium phosphate bioceramics with high purity, suitable size and low level of impurities with certain modifications in reaction parameters. Hence the current work deals with the preparation of synthetic calcium phosphate nanoceramics in relatively shorter time period compared to traditional methods with better product yield. The obtained nanoproduct was thermally stable up to 1000°C (without any traces of beta-TCP as a by product) with high purity level closer to that of bone and teeth, planning to get improved and further effective ceramic materials for use as powders or as nanocomposites in future efforts. The smaller reaction time with high product yield and suitable particle size compared to that reported in the literature would make these nano-HA particles more promising materials for use in bone replacement applications.

About the authors

Aneela Anwar

Aneela Anwar completed her PhD from University College London, UK, on Islamic Development Bank Merit Scholarship. She returned to her organization, University of Engineering and Technology and has been chairing the basic sciences department. She has presented her quality research work at various national and international podia. The nature of her work, supreme presentation skills and innovation ideas had been appreciated much. She holds a patent besides various research publications. Her research mainly deals with the investigation of novel synthesis methodologies and analysis of various high purity nanoscale biomedical materials as medical device for hospitals/orthopaedic surgeon and research field.

Qudsia Kanwal

Qudsia Kanwal received her PhD degree from University of Punjab Pakistan as an HEC scholar. She worked as an assistant professor in Lahore College for women university Lahore and as visiting Faculty in University of Engineering and Technology, Lahore. Now she is working as an assistant professor in the University of Lahore. Her research interests are biopesticides synthesis, green chemistry and nanochemistry.

Samina Akbar

Samina Akbar is an Assistant Professor of Chemistry at the University of Engineering and Technology Lahore, KSK campus, Pakistan. Her research interests embrace the use of Lyotropic Liquid Crystals as a template for the production of highly ordered nanostructured platinum materials. She is investigating the fabrication and characterization of nanostructured materials. These materials exhibit very high surface area, high conductivity, and chemical stability which make them ideal for use in the next generation energy storage and energy conversion devices.

Aisha Munawar

Aisha Munawar completed her Masters (1998) and MPhil studies in inorganic Analytical chemistry from the Quaide-Azam University in 2000. She joined the Department of Chemistry, University of Engineering and Technology, Lahore, in 1999 as a lecturer. Later she completed her doctorate studies at The University of Hamburg, in 2012. Her research interests are proteomics, peptide isolation and characterization, snake venom, inorganic chemistry and biomaterials.

Arjumand Durrani

Arjumand Iqbal Durrani did her MSc and MPhil in chemistry from the University of Engineering and Technology, Lahore and University of Punjab, Lahore, respectively. She has done PhD from University of Vienna, Austria, in the field of analytical and food chemistry. She has research interest in the field of analytical chemistry, food chemistry, nanotechnology and environmental chemistry. She has more than 12 years of teaching experience both at graduate and post-graduate level.

Masood Hassan Farooq

Masood Hassan Farooq is working as an Assistant Professor of Physics in the University of Engineering and Technology, Lahore since September 2015. He has joined the Laboratory of Eco-Materials and Sustainable Energy Post-Doct research of The Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Urumqi, P. R. China (2013–2015). He worked on the fabrication of advanced functional materials and their environmental applications. He got the doctorate degree in Applied Physics from the University of Science and Technology Beijing (USTB), P. R. China (2010–2013). He has published 23 scientific articles in different journals, i.e. Crystal Engineering Communication, RSC Advance, Material Letters having IF above 45.

References

[1] Kokubo T. Bioceramics and their clinical applications, Woodhead Publishing and Maney Publishing: Cambridge, England, on behalf of Institute of Materials, Minerals & Mining, 2008.Search in Google Scholar

[2] Johansson P, Jimbo R, Kozai Y, Sakurai T, Kjellin P, Currie F, Wennerberg A. Nanosized hydroxyapatite coating on PEEK implants enhances early bone formation: a histological and three-dimensional investigation in rabbit bone. Materials 2015, 8, 3815–3830.10.3390/ma8073815Search in Google Scholar PubMed PubMed Central

[3] Uskoković V, Uskoković DP. Nanosized hydroxyapatite and other calcium phosphates: chemistry of formation and application as drug and gene delivery agents. J. Biomed. Mater. Res. B Appl. Biomater. 2011, 96, 152–191.10.1002/jbm.b.31746Search in Google Scholar PubMed

[4] Hench LL. Bioceramics. J. Am. Ceram. Soc. 1998, 81, 1705.10.1111/j.1151-2916.1998.tb02540.xSearch in Google Scholar

[5] Hench LL. The challenge of orthopaedic materials. Curr. Orthopaedics 2000, 14, 7.10.1054/cuor.1999.0074Search in Google Scholar

[6] Agrawal K, Singh G, Puri D, Prakash S. Synthesis and characterization of hydroxyapatite powder by sol-gel method for biomedical application. J. Miner. Mater. Characterization Eng. 2011, 10, 27–734.10.4236/jmmce.2011.108057Search in Google Scholar

[7] Katti KS. Biomaterial in total joint replacement. Colloid. Surfaces B 2004, 39, 133.10.1016/j.colsurfb.2003.12.002Search in Google Scholar PubMed

[8] Guler H, Gundogmaz G, Kurtulus F, Celik G, Gacanoglu S. Solid state synthesis of calcium borohydroxyapatite. Solid State Sci. 2011, 13, 1916.10.1016/j.solidstatesciences.2011.08.016Search in Google Scholar

[9] Sopyan L, Singh R, Hamdi M. Synthesis of nano sized hydroxyapatite powder using sol-gel technique and its conversion to dense and porous bodies. Ind. J. Chem. 2008, 47, 1626–1631.Search in Google Scholar

[10] Hench LL, West JK. The sol-gel process. Chem. Rev. 1990, 90, 33.10.1021/cr00099a003Search in Google Scholar

[11] Jokanović, V, Spasić AM, Uskoković D. Designing of nanostructured hollow TiO2 spheres obtained by ultrasonic spray pyrolysis. J. Colloid Interface Sci. 2004, 278, 342–352.10.1016/j.jcis.2004.06.008Search in Google Scholar PubMed

[12] Wang YJ, Lai C, Wei K, Chen X, Ding Y, Wang ZL. Investigations on the formation mechanism of hydroxyapatite synthesized by the solvothermal method. Nanotechnology 2006, 17, 4405.10.1088/0957-4484/17/17/020Search in Google Scholar

[13] Darr JA, Guo ZX, Raman V, Bououdina M, Rehman IU. Metal organic chemical vapour deposition (MOCVD) of bone mineral like carbonated hydroxyapatite coatings. Chem. Commun.(Camb) 2004, 696–697. 10.1039/B312855P.Search in Google Scholar

[14] Afshar A, Ghorbani M, Ehsani N, Saeri MR, Sorrell CC. Some important factors in the wet precipitation process of hydroxyapatite. Mater. Design 2003, 24, 197.10.1016/S0261-3069(03)00003-7Search in Google Scholar

[15] Oliveira JM, Costa SA, Leonor IB, Malafaya PB, Mano JF, Reis RL. Novel hydroxyapatite/carboxymethylchitosan composite scaffolds prepared through an innovative “autocatalytic” electroless coprecipitation route. J. Biomed. Mater. Res. A 2009, 88, 470–480.10.1002/jbm.a.31817Search in Google Scholar

[16] Hench LL, Wilson J. An Introduction to Bioceramics,Advanced Series in Ceramics, Vol.1, World Scientific Publishing, 1993.10.1142/2028Search in Google Scholar

[17] Liu C, Huang Y, Shen W, Cui J. Kinetics of HA precipitation at pH 10-1. Biomaterials 2001, 22, 301–306.10.1016/S0142-9612(00)00166-6Search in Google Scholar

[18] Raynaud S, Champion E, Bernasche-Assollant D, Thomas P. Calcium phosphate apatites with variable Ca/P atomic ratio I. Synthesis, characterization and thermal stability of powder. Biomaterials 2002, 2, 1065–1072.10.1016/S0142-9612(01)00218-6Search in Google Scholar

[19] Ahn E, Gleason NJ, Nakahira A, Ying JY. Nanostructure processing of HA based bioceramics, Nano Lett. 2001, 1, 149–153.10.1021/nl0055299Search in Google Scholar

[20] Lorenzo LMR, Regi MV, Ferreira JMF. Fabrication of HA bodies by uniaxial pressing from a precipitated powder. Biomaterials 2001, 22, 583–588.10.1016/S0142-9612(00)00218-0Search in Google Scholar

[21] Atkins P, De Paula J, Atkins J. Physical Chemistry, the Investigation of Structure, vol. 9. Oxford University Press: Oxford, UK, 2010, pp. 699–708.Search in Google Scholar

[22] Venkatasubbu GD, Ramasamy S, Ramakrishnan V, Kumar J. Nanocrystalline hydroxyapatite and zinc-doped hydroxyapatite as carrier material for controlled delivery of ciprofloxacin. 3 Biotech. 2011, 1, 173–186.10.1007/s13205-011-0021-9Search in Google Scholar PubMed PubMed Central

[23] Penel G, Leroy G, Rey C, Bres E. MicroRaman spectral study of the PO4 and CO3 vibrational modes in synthetic and biological apatites. Calcified Tissue Int. 1998, 63, 475–481.10.1007/s002239900561Search in Google Scholar PubMed

[24] Ciobanu CS, Iconaru SL, Massuyeau F, Constantin LV, Costescu A, Predoi D. Synthesis, structure, and luminescent properties of europium-doped hydroxyapatite nanocrystalline powders. J. Nanomater. 2012, 2012, 9.10.1155/2012/942801Search in Google Scholar

[25] Costescu A, Pasuk I, Ungureanu F, Dinischiotu A, Costache M, Huneau F, Galaup S, Le Coustumer P, Predoi D. Physico-chemical properties of nano-sized hexagonal hydroxyapatite powder synthesized by sol-gel. Dig. J. Nanomater. Biostruct. 2010, 5, 989–1000.Search in Google Scholar

[26] Lu HB, Campbell CT, Graham DJ, Ratner BD. Surface characterization of hydroxyapatite and related calcium phosphates by XPS and TOF-SIMS. Anal. Chem. 2000, 72, 2886–2894.10.1021/ac990812hSearch in Google Scholar PubMed

[27] Mahbole M, Aiyer R, Ramakrishina C, Sreedhar B, Khairnar R. Synthesis, characterization and gas sensing property of hydroxyapatite ceramic. Bull. Mater. Sci. 2005, 28, 535–545.10.1007/BF02706339Search in Google Scholar

[28] Stanić V, Dimitrijević S, Antić-Stanković J, Mitrić M, Jokić B, Plećaš IB, Raićević S. Synthesis, characterization and antimicrobial activity of copper and zinc-doped hydroxyapatite nanopowders. Appl. Surf. Sci. 2010, 256, 6083–6089.10.1016/j.apsusc.2010.03.124Search in Google Scholar

[29] Thian E, Konishi T, Kawanobe Y, Lim P, Choong C, Ho B, Aizawa M. Zinc-substituted hydroxyapatite: a biomaterial with enhanced bioactivity and antibacterial properties. J. Mater. Sci. Mater. Med. 2013, 24, 437–45.10.1007/s10856-012-4817-xSearch in Google Scholar PubMed

[30] Nayak AK. Hydroxyapatite synthesis methodologies: an overview. Int. J. ChemTech Research 2010, 2, 903–907.Search in Google Scholar

Received: 2016-4-12
Accepted: 2016-4-30
Published Online: 2016-7-12
Published in Print: 2017-4-1

©2017 Walter de Gruyter GmbH, Berlin/Boston

This article is distributed under the terms of the Creative Commons Attribution Non-Commercial License, which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

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https://doi.org/10.1515/ntrev-2016-0020
Keywords for this article
bioceramics; hydroxyapatite (HA); nanorods; X-ray diffraction
Creative Commons
BY-NC-ND 3.0

Articles in the same Issue

  1. Frontmatter
  2. In this issue
  3. Research highlights
  4. Synthesis and characterization of pure and nanosized hydroxyapatite bioceramics
  5. Nanotechnology as a proxy to capture regional economic development? New findings from the European Union Framework Programmes
  6. Reviews
  7. Does nanobiotechnology create new tools to combat microorganisms?
  8. Gelatin nanoparticles: a potential candidate for medical applications
  9. Research highlight
  10. Investigation on hemolytic effect of poly(lactic co-glycolic) acid nanoparticles synthesized using continuous flow and batch processes
  11. Nanotechnology education
  12. An acoustic teaching model illustrating the principles of dynamic mode magnetic force microscopy
  13. Reviews
  14. Upconversion nanoparticles for bioimaging
  15. Antibacterial potential of nanocomposite-based materials – a short review
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