Morphology Tailoring of Hydroxyapatite Nanoparticles by Hydrothermal Processing with Amino Acids

2007 ◽  
Vol 280-283 ◽  
pp. 1533-1536 ◽  
Author(s):  
Wei Min Gao ◽  
Qun Yan Li ◽  
Cheng Xiang Ruan ◽  
Yun Fa Chen

Hydroxyapatite (HAp) was synthesized in the presence of a variety of amino acids in order to investigate the effect of amino acid on the morphology of HAp obtained by homogeneous precipitation and hydrothermal treating. In the results of X-ray diffraction analysis, HAp synthesized in the presence of some amino acids showed different crystallinity compared with HAp synthesized in the absence of amino acid. The results of Fourier transform infrared spectroscopy suggested the adsorption of these amino acids on HAp. Microphotographs of transmission electron microscope showed that the size and morphology of HAp adsorbed amino acids changed significantly. Collectively, this study suggests that the morphology and the crystallinity of synthesized HAp are different owing to the variation of amino acids in the synthesizing condition.

2007 ◽  
Vol 336-338 ◽  
pp. 2096-2099 ◽  
Author(s):  
Wei Min Gao ◽  
Cheng Xiang Ruan ◽  
Yun Fa Chen

Hydroxyapatite nanoparticles were synthesized in the presence of two kinds of acidic amino acids in order to investigate the effects of acidic amino acids on the morphology of hydroxyapatite obtained by homogeneous precipitation and hydrothermal treating. The results of X-ray diffraction analysis and microphotographs of transmission electron microscope showed that the morphology of hydroxyapatite nanoparticles changed significantly only with aspartic acid. Hydroxyapatite synthesized with aspartic acid showed smooth flake-like morphology at pH= 11 and flake-like morphology with stripes at pH= 8. However, hydroxyapatite synthesized in the present of glutamic acid showed rod-like morphology at both pH values. Variation in the morphology of nanoparticles could be consistent with the difference in the affinity of amino acids binding at the hydroxyapatite crystal surface. The adsorption process was revealed by computer simulation of molecular mechanics using energy minimizing method.


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.


2012 ◽  
Vol 1481 ◽  
pp. 45-52
Author(s):  
A. Medina ◽  
L. Béjar ◽  
G. Herrera-Pérez

ABSTRACTMagnesium hydroxide (Mg(OH)2) nanoparticles were synthesized by chemical precipitation synthesis method. The influence of the nano-sized Mg(OH)2 on the structural modification was evaluated. The formation of Mg(OH)2 crystals were evaluated by Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA). The particle size and morphology of Mg(OH)2was confirmed by high resolution transmission electron microscopy (HRTEM). The crystalline structure of nanoparticles was characterized by fast Fourier transform (FFT) and X-Ray diffraction (XRD), like analytical tools.


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.


2016 ◽  
Vol 35 (6) ◽  
pp. 559-566 ◽  
Author(s):  
Elaheh Esmaeili ◽  
Mohammad Sabet ◽  
Masoud Salavati-Niasari ◽  
Kamal Saberyan

AbstractPbS nanostructures were synthesized successfully via hydrothermal approach with a new precursor. The products were characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and UV–Vis diffuse reflectance spectroscopy (DRS). The effect of different sulfur sources were investigated on product size and morphology.


Clay Minerals ◽  
2004 ◽  
Vol 39 (4) ◽  
pp. 391-404 ◽  
Author(s):  
J. E. F. C. Gardolinski ◽  
G. Lagaly ◽  
M. Czank

AbstractKaolinite and synthetic γ-Al(OH)3 (gibbsite or hydrargillite) were reacted with phenylphosphonic, phenylphosphinic and 2-nitrophenol-4-arsonic acids. The products were studied by powder X-ray diffraction, transmission electron microscopy/selected area electron diffraction/ energy dispersive X-ray/Fourier transform infrared and simultaneous thermogravimetric/differential thermal analysis. The acids were not intercalated but, instead, easily destroyed the structure of the minerals. Lamellar Al phenylphosphonate and aluminium phenylphosphinate and phenylarsonate with polymeric linear-chain structures were formed from kaolinite. The reaction between gibbsite and the same acids yielded almost identical products. No evidence of formation of grafted kaolinite derivatives after the reaction with phenylphosphonic acid was found.


2014 ◽  
Vol 602-603 ◽  
pp. 19-22 ◽  
Author(s):  
Lin Qiang Gao ◽  
Hai Yan Chen ◽  
Zhen Wang ◽  
Xin Zou

Nanoscale LiTaO3 powders with perovskite structure were synthesized using the solvothermal technique with glycol as solvent at 240°C for 12h. The powders were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). XRD was used to elucidate room temperature structures using Rietveld refinement. The powders were pure single pervoskite phase with high crystallinity. FESEM and TEM were used to determine particle size and morphology. The average LiTaO3 grain size was estimated to be < 200nm, and TEM images indicated that LiTaO3 particles had a brick-like morphology. In addition, the effect of the temperature on the LiTaO3 power characterisitics was also detailed studied.


Biomimetics ◽  
2021 ◽  
Vol 6 (4) ◽  
pp. 70
Author(s):  
Dmitry Goloshchapov ◽  
Vladimir Kashkarov ◽  
Kirill Nikitkov ◽  
Pavel Seredin

Differences in the surface interactions of non-stoichiometric nanocrystalline B-type carbonate-substituted hydroxyapatite (n-cHAp) with the amino acids L-Lysine hydrochloride (L-LysHCl) and L-Arginine hydrochloride (L-ArgHCl) in acidic and alkaline media were determined using structural and spectroscopic analysis methods. The obtained data confirm that hydroxyapatite synthesized using our technique, which was used to develop the n-cHAp/L-LysHCl and n-cHAp/L-ArgHCl composites, is nanocrystalline. Studies of molecular composition of the samples by Fourier transform infrared spectroscopy under the change in the charge state of L-Lysine in environments with different alkalinity are consistent with the results of X-ray diffraction analysis, as evidenced by the redistribution of the modes’ intensities in the spectra that is correlated with the side chains, i.e., amide and carboxyl groups, of the amino acid. During the formation of a biomimetic composite containing L-Lysine hydrochloride and n-cHAp, the interaction occurred through bonding of the L-Lysine side chain and the hydroxyl groups of hydroxyapatite, which created an anionic form of L-Lysine at pH ≤ 5. In contrast, in biocomposites based on L-Arginine and n-cHAp, the interaction only slightly depends on pH value, and it proceeds by molecular orientation mechanisms. The X-ray diffraction and infrared spectroscopy results confirm that changes in the molecular composition of n-cHAp/L-ArgHCl biomimetic composites are caused by the electrostatic interaction between the L-ArgHCl molecule and the carbonate-substituted calcium hydroxyapatite. In this case, the bond formation was detected by Fourier transform infrared (FTIR) spectroscopy; the vibrational modes attributed to the main carbon chain and the guanidine group of L-Arginine are shifted during the interaction. The discovered interaction mechanisms between nanocrystalline carbonate-substituted hydroxyapatite that has physicochemical properties characteristic of the apatite in human dental enamel and specific amino acids are important for selecting the formation conditions of biomimetic composites and their integration with the natural dental tissue.


2015 ◽  
Vol 19 (56) ◽  
Author(s):  
Muflihatun ◽  
Siti Shofiah ◽  
Edi Suharyadi

Nanopartikel Nikel Ferit (NiFe2O4) telah disintesis dengan metode kopresipitasi dengan memvariasi konsentrasi NaOH dan suhu sintesis. Struktur kristal, ukuran partikel, dan morfologi dari sampel dianalisa menggunakan X-ray diffraction (XRD) dan transmission electron microscopy (TEM). Ukuran butir pada konsentrasi NaOH 3, 5, dan 10 M masing-masing adalah 5,7; 4,3; dan 4,2 nm, sedangkan pada suhu 60, 80, dan 150°C berturut-turut adalah 4,2; 4,9; dan 5,5 nm. Analisa fourier transform infrared (FTIR) menunjukkan dua puncak serapan pada rentang ~400-600 cm-1 yang terkait dengan site oktahedral dan tetrahedral pada struktur NiFe2O4. Sifat magnetik NiFe2O4 hasil analisa vibrating sample magnetometer (VSM) menunjukkan bahwa sampel berperilaku ferromagnetik dengan nilai koersivitasnya pada rentang 42-47 Oe. Sampel dengan variasi konsentrasi NaOH, koersivitasnya cenderung menurun dengan menurunnya ukuran partikel. Sementara sampel dengan variasi suhu, semakin kecil ukuran partikel, koersivitasnya cenderung meningkat. Pada 15 kOe, nilai magnetisasi terbesar (6,17 emu/g) diperoleh pada sampel dengan rasio fasa α-Fe2O3 paling rendah.


2018 ◽  
Vol 73 (7) ◽  
pp. 467-480 ◽  
Author(s):  
Eva Pušavec Kirar ◽  
Uroš Grošelj ◽  
Amalija Golobič ◽  
Franc Požgan ◽  
Sebastijan Ričko ◽  
...  

Abstract [3+2] cycloadditions of ynones derived from glycine and (S)-alanine and some other dipolarophiles with azomethine imines, nitrile oxides, diazoacetate, and azidoacetate were studied. The dipolarophiles were obtained from α-amino acids, either by the reduction of the carboxy function with ethynylmagnesium bromide or by propiolation of the amino function. Cu-catalyzed cycloadditions of ynones to azomethine imines were regioselective and gave the expected cycloadducts as inseparable mixtures of diastereomers. In some instances, further oxidative hydrolytic ring-opening took place to afford 3,3-dimethyl-3-(1H-pyrazol-1-yl)propanoic acids. Acid-catalyzed cycloadditions of 3-butenone were also regioselective and provided mixtures of diastereomeric cycloadducts, which were separated by chromatography. In the reactions of title ynones with alkyl diazoacetates, in situ-formed benzonitrile oxides, and tert-butyl azidoacetate, all cycloadducts were obtained as single regioisomers. The structures of all novel compounds were established by nuclear magnetic resonance and X-ray diffraction.


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