Synthesis of Chicken’s Eggshells-Based β-Tricalcium Phosphate Bioceramics

2015 ◽  
Vol 1112 ◽  
pp. 458-461
Author(s):  
Kiagus Dahlan ◽  
Nur Aisyah Nuzulia

The use of bioceramics for orthopedic and dental application nowadays increases due to their good biocompatibility and osteoconductivity. β-tricalcium phosphate (β-TCP) bioceramics which have excellent biodegradation properties have been in use quite extensively. This paper reports the synthesis of β-TCP bioceramics from precipitation of calcined chicken’s eggshells and phosphoric acid (H3PO4). Chicken’s eggshells were calcined at 1000°C for 5 hours to form calcium oxide (CaO). Various molarities of CaO and H3PO4, between 0.4 M and 2.4 M, were used in this experiment with the Ca:P ratio was kept 1.5:1. After precipitation, the samples were filtered and heated at a sintering temperature of 1000°C for 7 hours. The X Ray Diffraction profile showed that the patterns were affected by the molarity. The patterns of 1.2 M CaO/0.8 M H3PO4 samples showed pure β-TCP, while those of 0.6 M CaO/0.4 M H3PO4 and 2.4 M CaO/1.6 M H3PO4 samples showed the presence of hydroxyapatite and octa calcium phosphate. These findings were also supported by Fourier transform infrared spectra. The purity of the samples shown by the atomic absorption spectroscopy resulted in Ca:P ratio of 1.48:1 which is very closed to that of standard β-TCP bioceramics.

2012 ◽  
Vol 727-728 ◽  
pp. 1164-1169 ◽  
Author(s):  
Mônica Beatriz Thürmer ◽  
Rafaela Silveira Vieira ◽  
Juliana Machado Fernandes ◽  
Wilbur Trajano Guerin Coelho ◽  
Luis Alberto Santos

Calcium phosphate cements have bioactivity and osteoconductivity and can be molded and replace portions of bone tissue. The aim of this work was to study the obtainment of α-tricalcium phosphate, the main phase of calcium phosphate cement, by wet reaction from calcium nitrate and phosphoric acid. There are no reports about α-tricalcium phosphate obtained by this method. Two routes of chemical precipitation were evaluated and the use of two calcinations temperatures to obtain the phase of cement. The influence of calcination temperature on the mechanical properties of cement was evaluated. Cement samples were characterized by particle size analysis, X-ray diffraction, mechanical strength and scanning electron microscopy. The results demonstrate the strong influence of synthesis route on the crystalline phases of cement and the influence of concentration of reactants on the product of the reaction, as well as, on the mechanical properties of cement.


2007 ◽  
Vol 561-565 ◽  
pp. 1553-1556 ◽  
Author(s):  
Sen Yang ◽  
Hau Chung Man

A layer of bioceramic HA was coated on laser gas nitrided and grit-blasted pure Ti substrates using plasma-spraying technique, respectively. X-ray diffraction analysis showed that the microstructures of the coating were mainly composed of HA, amorphous calcium phosphate and some minute phases of tricalcium phosphate, tetracalcium phosphate and calcium oxide. The experimental results showed that the 3-D TiN dendritic scaffold structure produced on the surface of pure Ti using laser gas nitriding technique in advance could anchor the HA coating and improved the interfacial adherence significantly as compared with those on the grit blasted surfaces.


2016 ◽  
Vol 698 ◽  
pp. 8-12 ◽  
Author(s):  
Shinichi Furusawa ◽  
Yohei Minami

In this study, KAlSi3O8 was synthesized by a solid-phase reaction at 900, 1000 and 1100 °C, using K2CO3, Al2O3 and SiO2 as the starting materials. The powder X-ray diffraction profile of the compound thus prepared was confirmed to contain a mixture of crystalline and glass phases. In addition, a higher sintering temperature of greater than 1000 °C possibly led to the decrease in the crystalline phase. From the temperature dependence of dc conductivity, activation energies for ionic transport were estimated to be 0.79–0.84 eV. The frequency-dependence of the real part of electrical conductivity suggests that the mechanism of ionic transport in the dispersion region possibly depends on the crystallinity of KAlSi3O8.


2007 ◽  
Vol 14 (01) ◽  
pp. 71-77 ◽  
Author(s):  
H. LIANG ◽  
Y. HUANG ◽  
F. HE ◽  
H. F. DING ◽  
Y. Z. WAN

Modification of bioceramics by ion implantation of magnesium ( Mg ) is of interest as Mg is the fourth abundant cation in the human body. In this work, magnesium was ion-implanted into a ZrO 2 based bioceramic stabilized with Y 2 O 3 and Al 2 O 3. Both Mg -implanted and unimplanted samples were soaked in a simulated body fluid (SBF) for a period of time. The deposits on the surface of various samples were characterized with scanning electron microscope (SEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). We find that the Mg -implanted ZrO 2 shows better bioactivity than the plain bioceramic. These results indicate that Mg -implantation can improve the bioactivity of the ZrO 2 based bioceramic. Mechanisms governing the improvement are discussed in this paper.


Author(s):  
Alessandra Giuliani ◽  
Maria Laura Gatto ◽  
Luigi Gobbi ◽  
Francesco Guido Mangano ◽  
Carlo Mangano

Purpose: Several studies showed that the sintering temperature of 1250 °C could affect the formation of α-Ca3(PO4)2, which is responsible for the reduction of the hardness value of biphasic calcium phosphate biocomposites, but they did not evaluate the inference of the sintering time at peak temperature on transition of β-Ca3(PO4)2 to α-Ca3(PO4)2. This analysis explored, in an innovative way, inferences and correlations between volumetric microstructure, mechanical properties, sintering temperature, and time at peak temperature in order to find the best sintering conditions for biphasic calcium phosphate composites grafted in severe alveolar bone defects. Methods: Sintered biphasic calcium phosphates (30%-hydroxyapatite/70%-tricalcium phosphate) were tested by microCT imaging for the 3D morphometric analysis, by compressive loading to find their mechanical parameters, and by X-ray diffraction to quantify the phases via Rietveld refinement for different sintering temperatures and times at the peak temperature. Data were analysed in terms of statistical inference using Pearson’s correlation coefficients. Results: All the studied scaffolds closely mimicked the alveolar organization of the jawbone, independently on the sintering temperatures and times; however, mechanical testing revealed that the group with peak temperature, which lasted for 2 hours at 1250 °C, showed the highest strength both at the ultimate point and at fracture point. Conclusion: The good mechanical performances of the group with peak temperature, which lasted for 2 hours at 1250 °C, is most likely due to the absence of the α-Ca3(PO4)2 phase, as revealed by X-ray diffraction. However, we detected its presence after sintering at the same peak temperature for longer times, showing the time-dependence, combined with the temperature-dependence, of the β-Ca3(PO4)2 to α-Ca3(PO4)2 transition.


2016 ◽  
Vol 1 (2) ◽  
Author(s):  
Veni Dayu Putri

<p><strong>ABSTRAK</strong></p><p><strong> </strong></p><p>Pembuatan lapisan tipis kalsium fosfat dari kalsium nitrat tetrahidrad (Ca(NO<sub>3</sub>)<sub>2</sub>.4H<sub>2</sub>O) sebagai prekursor kalsium dan asam fosfat (H<sub>3</sub>PO<sub>4</sub>) sebagai <em>prekursor</em> fosfat dengan variasi perbandingan mol Ca/P 1.50 , 1.60 , 1.67 , 1.70 dan 1.80 melalui metode sol-gel telah dilakukan. Sol yang didapat dibakar pada suhu 1000<sup>o</sup>C sehingga terbentuk powder kalsium fosfat berwarna putih. Powder yang didapat dianalisis menggunakan Fourier Transform Infra Red Spectroscopy (FTIR), X-Ray Diffraction (XRD) dan Scanning Electron Microscopy (SEM). Analisis FTIR menunjukkan adanya serapan gugus PO<sub>4</sub><sup>3-</sup>, O-H, H<sub>2</sub>O, CO<sub>2</sub>, dan P<sub>2</sub>O<sub>7</sub><sup>4-</sup>. Difraksi sinar-X dari powder yang terbentuk memberikan puncak pada sudut 2θ yang berbeda yaitu <em>Calsium Pyrophospate</em> (Ca<sub>2</sub>P<sub>2</sub>O<sub>7</sub>) dan <em>Hydroxyapatite</em> HAP (Ca<sub>10</sub>(PO<sub>4</sub>)<sub>6</sub>(OH)<sub>2 </sub>pada perbandingan molar Ca/P 1.80 . Analisis SEM menghasilkan <em>Hydroxyapatite </em>dan <em>Calsium Pyrophospate </em>dengan distribusi partikel yang tidak merata dan berbentuk <em>spheric</em>. Proses pelapisan dilakukan pada plat kaca yaitu pada perbandingan mol Ca/P 1.80 menggunakan metode dip-coating dan kemudian dipanaskan pada suhu 400<sup>o</sup>C. Hasil analisa XRD pada lapisan kalsium fosfat memperlihatkan bahwa senyawa yang terbentuk berbentuk amorf. Sedangkan analisis menggunakan SEM memperlihatkan bahwa lapisan tipis kalsium fosfat memiliki morfologi permukaan yang halus, rapat, homogen dan berbentuk <em>speric</em>.</p><p> </p><p>         <strong><em>Kata kunci</em></strong> : kalsium fosfat, <em>hydroxyapatite</em>, <em>dip-coating</em>, metode sol-gel</p><p> </p><p><strong>ABSTRACT</strong></p><p align="center"><strong> </strong></p><p><em>Preparation a thin layer of calcium phosphate using tetrahidrad calcium nitrate (Ca(NO<sub>3</sub>)<sub>2</sub>.4H<sub>2</sub>O) as a precursor of calcium and phosphoric acid (H<sub>3</sub>PO<sub>4</sub>) as a precursor of phosphate with a variation of the mole ratio Ca/P 1.50; 1.60, 1.67, 1.70 and 1.80 through the sol-gel method have been done. Sol obtained burned at a temperature of 1000<sup>o</sup>C to form white powder of calcium phosphate. Powder obtained were analyzed using Fourier Transform Infra Red Spectroscopy (FTIR), X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). FTIR analysis showed absorption PO<sub>4</sub><sup>3-</sup> group,  O-H, H<sub>2</sub>O, CO<sub>2</sub>, and P<sub>2</sub>O<sub>7</sub><sup>4-</sup>. X-ray diffraction from powder formed providing a peak at an angle 2θ different namely Calcium Pyrophospate (Ca<sub>2</sub>P<sub>2</sub>O<sub>7</sub>) and Hydroxyapatite HAP (Ca<sub>10</sub>(PO<sub>4</sub>)<sub>6</sub>(OH)<sub>2</sub>) at a molar ratio of Ca/P 1.80. Analysis of SEM produces Hydroxyapatite and Calcium Pyrophospate with particle distribution is uneven and shaped spheric. The coating process performed on glass plates with mole ratio of Ca/P 1.80 using a dip-coating and then heated at a temperature of 400<sup>o</sup>C. XRD analysis on a layer of calcium phosphate showed that the compound formed shaped amorphous. While using SEM analysis showed the morphology of thin layer of calcium phosphate are smooth, dense, homogeneous and shaped speric.</em></p><p><em> </em></p><p><em>         <strong>Keywords :</strong> calcium phosphate, hydroxyapatite, dip-coating, sol-gel method</em></p>


2005 ◽  
Vol 284-286 ◽  
pp. 157-160 ◽  
Author(s):  
J.A. Delgado ◽  
I. Harr ◽  
Amisel Almirall ◽  
Sergio del Valle ◽  
Josep A. Planell ◽  
...  

In this work an injectable and self setting calcium phosphate/albumen foam is developed. The effect of both the amount of albumen and the particle size of the starting a-tricalcium phosphate (a-TCP) powder on the injectability of the cement paste is studied. X-ray diffraction (XRD) and infrared (IR) analysis of the samples reveal that the hydrolysis of a-TCP to calcium deficient hydroxyapatite (CDHA) is not affected by the addition of albumen. A foamed structure formed by spherical pores with diameters between 100 and 500 µm is observed by SEM. This porous structure is maintained after injection of the paste, although some deformation of the pores is produced due to the extrusion process. The injectability of the cements is increased by the presence of albumen as compared with cements prepared in the same conditions but without foaming agent.


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