Facile Refluxing Synthesis of Hydroxyapatite Nanoparticles

2015 ◽  
Vol 68 (8) ◽  
pp. 1293 ◽  
Author(s):  
Pakvipar Chaopanich ◽  
Punnama Siriphannon

Hydroxyapatite (HAp) nanoparticles were successfully synthesized from an aqueous mixture of Ca(NO3)2·4H2O and (NH4)2HPO4 by a facile single-step refluxing method using polystyrene sulfonate (PSS) as a template. The effects of reaction times, pH, and PSS concentration on the HAp formation were investigated. It was found that the crystalline HAp was obtained under all conditions after refluxing the precursors for 3 and 6 h. The longer refluxing time, the greater the crystallinity and the larger the crystallite size of the HAp nanoparticles. The HAp with poor crystallinity was obtained at pH 8.5; however, the well-crystallized HAp was obtained when reaction pH was increased to 9.5 and 10.5. In addition, the X-ray diffraction patterns revealed that the presence of PSS template caused the reduction of HAp crystallite size along the (002) plane from 52.6 nm of non-template HAp to 43.4 nm and 41.4 nm of HAp with 0.05 and 0.2 wt-% PSS template, respectively. Transmission electron microscopy images of the synthesized HAp revealed the rod-shaped crystals of all samples. The synthesized HAp nanoparticles were modified by l-aspartic acid (Asp) and l-arginine (Arg), having negative and positive charges, respectively. It was found that the zeta potential of HAp was significantly changed from +5.46 to –24.70 mV after modification with Asp, whereas it was +4.72 mV in the Arg-modified HAp. These results suggested that the negatively charged amino acid was preferentially adsorbed onto the synthesized HAp surface.

2007 ◽  
Vol 130 ◽  
pp. 203-206 ◽  
Author(s):  
Grzegorz Dercz ◽  
Lucjan Pająk ◽  
Krystian Prusik ◽  
Roman Pielaszek ◽  
Janusz J. Malinowski ◽  
...  

Wet gel obtained by sol-gel technique was dried in supercritical CO2 to prepare hydrated form of magnesium oxide. Calcination at 723 K under vacuum yielded nanocrystalline MgO aerogel. Structure studies were performed by X-ray diffraction, scanning and transmission electron microcopies. Electron microscopy images reveal rough, unfolded and ramified structure of solid skeleton. Specific surface area SBET was equal to 238 m2/g. X-ray pattern reveals the broadened diffraction lines of periclase, the only crystalline form of magnesium oxide. The gamma crystallite size distribution was determined using FW 5 4 / 5 1 M method proposed by R. Pielaszek. The obtained values of <R> and σ (measure of polydispersity) of particle size parameters are equal to 6.5 nm and 1.8 nm, respectively, whereas the average crystallite size estimated by Williamson-Hall procedure was equal to 6.0 nm. The obtained at Rietveld refinement Rwp, and S fitting parameters equal to 6.62% and 1.77, respectively, seem to be satisfactory due to the nanosize of MgO crystallites and because of the presence of amorphous phase.


2005 ◽  
Vol 888 ◽  
Author(s):  
Jin-Seo Noh ◽  
Dong-Seok Suh ◽  
Sang Mock Lee ◽  
Kijoon H. P. Kim ◽  
Woong-Chul Shin ◽  
...  

ABSTRACTConventional Ge2Sb2Te5 (GST) was modified by adding up a small amount of SiOx, using co-sputtering technique from multiple targets. The SiOx content was gradually increased by increasing the power applied to SiOx target, up to 8 volume percent. The sheet resistance of SiOx-containing GST exponentially increased, when the room-temperature-deposited samples were annealed at 300 °C. Transmission electron microscopy images revealed that no SiOx particulates were formed, which was confirmed by Gattan image filtering. It was indicated by x-ray diffraction patterns that the grain size of SiOx-containing GST is smaller than normal GST with lattice locally distorted at its crystalline state, suggesting that molecular SiOx is homogeneously distributed throughout the GST matrix. We observed that the crystallization temperature of SiOx-containing GST is gradually elevated by increasing the SiOx content, while the melting point decreased. These observations led to the reset current reduction, which is a critical requirement for the high density PRAM.


Clay Minerals ◽  
2010 ◽  
Vol 45 (2) ◽  
pp. 131-143 ◽  
Author(s):  
M. Bentabol ◽  
M. D. Ruiz Cruz ◽  
I. Sobrados

AbstractAl-lizardite has been synthesized under hydrothermal conditions (200ºC). Morphologically, Al-lizardite consists of thin platy particles ~400 Å wide and ~150 Å thick. Structurally, the X-ray diffraction patterns indicate that the 2H2 polytype is dominant, with cell parameters: a = 5.311(0.006) Å; c = 14.333 (0.013) Å and space group P63. High-resolution transmission electron microscopy images revealed, however, the presence of other polytypes and abundant stacking disorder. Chemically, Al-lizardite consists of a single population with average tetrahedral composition Si1.74Al0.26. In contrast to previously described Al-rich serpentines (amesite and Al-lizardite), this Al-lizardite is characterized by an asymmetrical Al distribution, with VIAl ≈0.70 and IVAl ≈0.25 atoms per formula unit.


Minerals ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 611
Author(s):  
Celia Marcos ◽  
María de Uribe-Zorita ◽  
Pedro Álvarez-Lloret ◽  
Alaa Adawy ◽  
Patricia Fernández ◽  
...  

Chert samples from different coastal and inland outcrops in the Eastern Asturias (Spain) were mineralogically investigated for the first time for archaeological purposes. X-ray diffraction, X-ray fluorescence, transmission electron microscopy, infrared and Raman spectroscopy and total organic carbon techniques were used. The low content of moganite, since its detection by X-ray diffraction is practically imperceptible, and the crystallite size (over 1000 Å) of the quartz in these cherts would be indicative of its maturity and could potentially be used for dating chert-tools recovered from archaeological sites. Also, this information can constitute essential data to differentiate the cherts and compare them with those used in archaeological tools. However, neither composition nor crystallite size would allow distinguishing between coastal and inland chert outcrops belonging to the same geological formations.


2014 ◽  
Vol 68 (8) ◽  
Author(s):  
Selvakumar Dhanasingh ◽  
Dharmaraj Nallasamy ◽  
Saravanan Padmanapan ◽  
Vinod Padaki

AbstractThe influence of cetyltrimethylammonium bromide and ethylene glycol on the size and dispersion of indium oxide nanoparticles prepared under hydrothermal conditions was investigated. The precursor compound, indium hydroxide, obtained by the hydrothermal method in the absence as well as the presence of cetyltrimethylammonium bromide, was converted to indium oxide by sintering at 400°C. The formation of nanoscale indium oxide upon sintering was ascertained by the characteristic infrared adsorption bands and X-ray diffraction patterns of indium oxide. Transmission electron microscopy and band gap values confirmed that the cetyltrimethylammonium bromide facilitated the formation of indium oxide nanoparticles smaller in size and narrower in distribution than those prepared without the assistance of cetyltrimethylammonium bromide.


2007 ◽  
Vol 7 (2) ◽  
pp. 525-529 ◽  
Author(s):  
Bo Zhou ◽  
Jun-Jie Zhu

A chemical co-reduction route in aqueous solution was developed to synthesize Bi100−xSbx alloys at room temperature. The hydrolyses of Bi(III) and Sb(III) were effectively avoided by selecting proper raw materials and coordinator. X-ray diffraction analysis indicated that the as-prepared Bi100−xSbx alloys were homogeneous and phase-pure, and the Bi/Sb ratios in the alloys were very close to those in the aqueous solutions. The transmission electron microscope observation showed that the as-prepared Bi100−xSbx (x = 0∼100) alloys were particles with a size of tens of nanometers. The selected area electron diffraction patterns confirmed the high crystallinity, the homogeneousness, and the composition controllability of as-prepared alloys. All these characters and the nanometer-scaled size of the alloys are believed to be beneficial to the thermoelectric property of the Bi100−xSbx alloys.


Author(s):  
Karthik Ramasamy ◽  
Weerakanya Maneerprakorn ◽  
Mohammad A. Malik ◽  
Paul O'Brien

Cobalt complexes of 1,1,5,5-tetramethyl-2,4-dithiobiuret, [Co{N(SCNMe 2 ) 2 } 3 ] ( 1 ), and 1,1,5,5-tetraisopropyl-2-thiobiuret, [Co{N(SOCN i Pr 2 ) 2 } 2 ] ( 2 ), have been synthesized and characterized. Both complexes were used as single-molecule precursors for the preparation of cobalt sulphide nanoparticles by thermolysis in hexadecylamine, octadecylamine or oleylamine. The powder X-ray diffraction pattern of as-prepared nanoparticles showed the hexagonal phase of Co 1− x S from complex 1 and mixtures of cubic and hexagonal Co 4 S 3 from complex 2 . Transmission electron microscopy images of material prepared from complex 1 showed spherical and trigonally shaped particles in the size range of 10–15 nm; whereas spheres, rods, trigonal prisms and pentagonally and hexagonally faceted crystallites were observed from complex 2 . This observation is the first of the Co 4 S 3 phase in a nanodispersed form.


2007 ◽  
Vol 7 (2) ◽  
pp. 634-640 ◽  
Author(s):  
M. Siliani ◽  
M. A. López-Manchado ◽  
J. L. Valentín ◽  
M. Arroyo ◽  
A. Marcos ◽  
...  

Novel millable polyurethane (PU)/organoclay nanocomposites have been successfully prepared by conventional transformation techniques. One natural (C6A) and two organically modified (C15A and C30B) montmorillonites have been used as clays for preparing PU nanocomposites. The optimum dispersion of nanofiller at a nanometer scale in PU matrix was confirmed by X-ray diffraction patterns and transmission electron microscopy. A substantial improvement of the PU properties by addition of only a small amount of organoclay was observed. It is worthy to note that the organoclays show a different interfacial interaction with the PU matrix, which was reflected in different macroscopic properties. Thus, C30B organoclay seems to react with PU chains to form covalent bonds, while C15Aonly interacts physically with PU chains. Mechanical and barrier properties are analyzed.


2012 ◽  
Vol 602-604 ◽  
pp. 227-230
Author(s):  
Tao Fan ◽  
Yan Rong Sun ◽  
Li Guo Ma

Spheroid hydroxyapatite nanoparticles were successfully prepared by titrating Ca(NO3)2•4H2O and (NH4)2HPO4 aqueous solution in the reverse microemulsion, which consists of mixed OP-10(surfactant), cyclohexane(oil phase), and isobutanol (cosurfactant).The structure and morphology of the prepared powders were characterized by means of X-ray diffraction (XRD) and transmission electron microscope (TEM). The optimum composition was investigated via the analysis of the aqueous solution conductivity, and the mechanism of aqueous reaction. The effect of the pH value and the amount of surfactant on the particle size were studied. The results indicate that the best conditions are which the concentration of OP-10 and isobutanol both are 0.2 M, when the water content is between 130 ml-250 ml,it results in pure nano-hydroxyapatite spheroid-like powders, and the water content is about 200 ml, whose diameters are 50 nm-80 nm, and good particle diameter distribution, the particle microstructure is homogeneous, good crystal structure and higher crystallinity.


2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
Wei-Lin Wang ◽  
Chia-Ti Wang ◽  
Wei-Chun Chen ◽  
Kuo-Tzu Peng ◽  
Ming-Hsin Yeh ◽  
...  

Ta/TaN bilayers have been deposited by a commercial self-ionized plasma (SIP) system. The microstructures of Ta/TaN bilayers have been systematically characterized by X-ray diffraction patterns and cross-sectional transmission electron microscopy. TaN films deposited by SIP system are amorphous. The crystalline behavior of Ta film can be controlled by the N concentration of underlying TaN film. On amorphous TaN film with low N concentration, overdeposited Ta film is the mixture ofα- andβ-phases with amorphous-like structure. Increasing the N concentration of amorphous TaN underlayer successfully leads upper Ta film to form pureα-phase. For the practical application, the electrical property and reliability of Cu interconnection structure have been investigated by utilizing various types of Ta/TaN diffusion barrier. The diffusion barrier fabricated by the combination of crystallizedα-Ta and TaN with high N concentration efficiently reduces the KRc and improves the EM resistance of Cu interconnection structure.


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