A novel batch hydrothermal method is indigenously developed to synthesize fine size, crystalline hydroxyapatite ha and titania doped hydroxyapatite tio2ha powders with distinct phase formation. The influence of precursor concentration, pressure, temperature and time of hydrothermal synthesis on the development of calcium hydroxyapatite structure has been analyzed. In this study, the effects of temperature on the hydrothermal synthesis of hydroxyapatite zeolite from blast furnace slag were investigated. Agarawal, satya prakash metallurgical and materials engineering department, indian institute of technology roorkee, india corrosponding author. Hydrothermal synthesis and biocompatibility study of highly crystalline carbonated hydroxyapatite nanorods caibao xue1, yingzhi chen2, yongzhuo huang2 and peizhi zhu1 abstract highly crystalline carbonated hydroxyapatite cha nanorods with different carbonate contents were synthesized by a novel hydrothermal method. Hydrothermal synthesis and biocompatibility study of highly. Hydroxyapatite hierarchically nanostructured porous hollow. Hydroxyapatite hap rods were synthesized from dicalcium phosphate anhydrous cahpo 4, dcpa and calcium carbonate caco 3 by the hydrothermal method from 120 to 180 c. In this work, hydroxyapatite nanorods were synthesized and characterized using a hydrothermal reaction with templates of fruit extracts in order to. Hydrothermal and solgel synthesis methods have been used to prepare nanoparticulate hydroxyapatite ha powders for detailed characterisation. Bioactivity measured after immersion in simulated body fluid.
Hydrothermal synthesis of hydroxyapatite j s earl, d j wood and s j milne institute for materials research, university of leeds, leeds, ls2 9jt, uk email. Such particles of nanorods were used to fabricate ha ceramic by using spark plasma sintering. Fe2o3, naytype zeolite and hydroxyapatite crystals at 100 to 160c and their properties are introduced. The ph value of the starting reaction solution and the temperature of hydrothermal treatment are the most signi. The term hydr othermal today includes methods which involve water at pressures from 1 atm several kilobars and high te mperatures from 100 10,000c. The obtained results show that it is possible to adjust the conditions of. Pdf hydrothermal synthesis of hydroxyapatite plates. There are several methods for synthesizing hydroxyapatite. Protein adsorption behavior of hydroxyapatite during. Jul 12, 2002 processing at phs lower than 9 can also result in the production of a calcium deficient hydroxyapatite. After hydrothermal treatment, carbonatesubstituted hap and tio2 anatase phases were formed in products using 1. Materials with enhanced physical and biological properties have been used. Hydrothermal synthesis and biocompatibility study of.
Hydrothermal synthesis and characterization of hydroxyapatite and fluorhydroxyapatite nanosize powders. Influence of hydrothermal synthesis parameters on the. Hydrothermal synthesis of hydroxyapatite rods sciencedirect. Compared to the formation of hap crystals via conventional. The prepared nanocrystalline hap was characterized for its phase purity and nanoscale.
These show the presence of secondary phases in the solgel powders which can be attributed to evaporative loss of. In this study, we synthesized the tio2modified hydroxyapatite hap with various morphologies by hydrothermal treatment using urea decomposition, at 160 oc for 6 h. The crystallinity and chemical structure of synthesized nanorods were studied by fourier transform infrared spectroscopy ftir, xray photoelectronic spectroscopy xps, xray diffraction xrd, raman spectroscopy, and transmission electron microscopy. Graduate school of environmental studies, tohoku university hydroxyapatite ha particles synthesized by hydrothermal treatment of octacalcium phosphate ocp particles were. The effects of ph and sintering temperature on the structural and morphological. The ctab as a template is used to regulate the nucleation and crystal growth. Gypsum powder could be completely converted to fine hap crystals 30. The following parameters of the obtained nanostructured hap were determined. Box 31787316, karaj, iran 2 center of excellence for production of advanced materials department of materials science and engineering. C for 6 hrs and organic oxide of titanium along with acidbase reflux is used as starting material for the synthesis of titania under. Hydrothermal synthesis of a mineralsubstituted hydroxyapatite nanocomposite material for fluoride removal from drinking water ammavasi nagaraj, a murugan a. Hydrothermal synthesis is a process that utilizes single or heterogeneous phase reactions in.
Pdf hydrothermal synthesis of hydroxyapatite hydrothermal. Hydroxyapatite ha is a synthetic ceramic which is used in numerous biomedical applications. In this study, the effect of microwave radiation on the hydrothermal synthesis of. Hydroxyapatite hap rods were synthesized from dicalcium phosphate anhydrous cahpo4, dcpa and calcium carbonate caco3 by the hydrothermal method from 120 to 180 c. Influence of hydrothermal synthesis parameters on the properties of hydroxyapatite nanoparticles hydroxyapatite hap nanoparticles of tunable diameter were obtained by the precipitation method at room temperature and by microwave hydrothermal synthesis mhs. Oct 01, 2007 hydroxyapatite hap rods were synthesized from dicalcium phosphate anhydrous cahpo 4, dcpa and calcium carbonate caco 3 by the hydrothermal method from 120 to 180 c. Leila montazeri 1,2, jafar javadpour 1,4, mohammad ali shokrgozar 2,4, shahin bonakdar 2 and sayfoddin javadian 3. The surface structure of hydroxyapatite hap particles during hydrothermal synthesis and their protein adsorption behavior was investigated. An attempt was conducted to synthesis nanocrystalline hydroxyapatite with a hydrothermal chemical method. Therefore, wet chemical reactions were investigated in solution at different temperatures by hydrothermal conditions aimed at hydroxyapatite ca 10 po 4 6 oh 2, hap synthesis. The effects of heating time and heating temperature on the products were investigated. Hydrothermal synthesis of hydroxyapatite with different morphologies. Hence, the chicken eggshells potentiallybecome a source of calcium inthe synthesis of ha. Hydrothermal synthesis of hydroxyapatite from calcium.
Hydrothermal synthesis an overview sciencedirect topics. Conclusions fine hydroxyapatite single crystals were synthesized by a hydrothermal method with caoh2 and cahpo4 2h2o as starting materials. After wet chemistry, hydrothermal techniques are the second most popular synthesis techniques for producing hydroxyapatite powders. Hydrothermal is one of t he best methods to produce pure fine oxide powders. In the 20th century, the hydrothermal technique for synthesis of materials was clearly identified as an important technology36 and using this technology various ceramic materials including hap can be synthesized. The effect of cano 3 2 4h 2 o and nh 4 2 hpo 4 primary solutions as the starting materials in the synthesis of a calcium phosphate phase was examined. Hydrothermal synthesis and characterization of hydroxyapatite from octacalcium phosphate natsuko ito, masanobu kamitakahara, setsuaki murakami, noriaki watanabe and koji ioku. Hydroxyapatite synthesis of hydroxyapatite powders. Furthermore, it is known that the reaction temperature during hydrothermal treatment can signi. C for 6 hrs and organic oxide of titanium along with acidbase reflux is used as starting material for the synthesis of titania under strong basic conditions.
Free fulltext pdf articles from hundreds of disciplines, all in one place hydrothermal synthesis and biocompatibility study of highly crystalline carbonated hydroxyapatite nanorods pdf paperity toggle navigation. The aim of this work was to investigate the influence of different reaction parameters on the properties of hydroxyapatite hap nanoparticles prepared by the hydrothermal method. A facile ureaassisted hydrothermal synthesis and systematic characterization of hydroxyapatite ha with calcium nitrate tetrahydrate and diammonium hydrogen phosphate as precursors are reported. Published 23 june 2010 2010 iop publishing ltd biomedical materials, volume 5, number 4. Pdf crystallographic study of hydrothermal synthesis of. Synthesis of hydroxyapatite bioceramic powder by hydrothermal method p. In 19 morey and niggli defined hydrothermal synthesis as in the hydrothermal method the components are subjected to the action of water, at temperatures generally near though often considerably above the critical temperature of water 370c in closed bombs, and therefore, under the corresponding high. Highly crystalline carbonated hydroxyapatite cha nanorods with different carbonate contents were synthesized by a novel hydrothermal method. Despite the high potential of slag utilization for the synthesis of these adsorbents, only two studies have been reported on the synthesis of hydroxyapatite using blast furnace slag 1,11. Synthesis and hydrothermal treatment of nanostructured.
Wet chemical synthesis of nanocrystalline hydroxyapatite. Hydroxyapatite hierarchically nanostructured porous hollow microspheres. From monetite plate to hydroxyapatite nanofibers by. The products were characterized by using ftir, xrd and tem. Hydrothermal synthesis by using creatine phosphate as an organic phosphorus source and application in drug delivery and protein adsorption. In this paper, spherical nanohydroxyapatite was synthesized by hydrothermal method. Furthermore, it is known that the reaction temperature during hydrothermal treatment can significantly affect the resulting crystalline phases and total crystallinity 14,15,25. However, its use is restricted in load bearing applications. A novel hydrothermal synthesis of nanohydroxyapatite from. In many cases, selforganized hierarchical nanostructures, such as nanoflowers and nanourchins, can be obtained spontaneously. Pdf hydrothermal synthesis of ultrafine hydroxyapatite. Hydrothermal synthesis is a very powerful tool for producing various functional nanomaterials of transitionmetal compounds, such as oxides, hydroxides, and sulfides.
An effective morphology control of hydroxyapatite crystals. Hydrothermal synthesis of hydroxyapatite with different. Hydroxyapatite nanoparticles with uniform morphologies and controllable size have been synthesized by lowtemperature hydrothermal method in the presence of cationic surfactant. In the present study, hydroxyapatite ha, ca5po43oh with different morphologies, such as nanorods, microspheres, hexagonal prisms, and hollow flowerlike structure, were synthesized via a facile hydrothermal route by adjusting reaction parameters. The hap particles were prepared by mixing calcium acetate solution and diammonium hydrogen phosphate solution by hydrothermal synthesis. Specimens were synthesized at different temperatures room temperature, 50, 90, 120, or 150 c. Blast furnace slag, an industrial byproduct, is emerging as a potential raw material to synthesize hydroxyapatite and zeolite. An effective morphology control of hydroxyapatite crystals via hydrothermal synthesis. Paper open access microwave treatment and ph influence. The literature data describe widely different experimental conditions for the hydrothermal synthesis of hap. These are wet method, dry method, hydrothermal method, alkoxide method, and flux method of various kinds of methods. Mar 17, 2005 hydrothermal synthesis has been used to produce hydroxyapatite ha particles with high crystallinity. Synthesis of spherical nanohydroxyapatite by hydrothermal.
The nucleation and growth of hap rods mainly occurred on dcpa particles, while some hap rods also. Fabrication of nanostructured hydroxyapatite via hydrothermal. Free fulltext pdf articles from hundreds of disciplines, all in one place hydrothermal synthesis and biocompatibility study of highly crystalline carbonated hydroxyapatite nanorods pdf. Hydrothermal synthesis of hydroxyapatite calcium nitrate tetrahydrate cano 3 24h 2. Synthesis of hydroxyapatite nanostructure by hydrothermal. Hydrothermal synthesis of hydroxyapatite from eggshell. Synthesis of nanocrystalline hydroxyapatite nanorods via. Supervised by akhiruddin maddu and yessie widya sari. Such synthesis routes can be practically expanded for making phase pure hap powders in industrial scale. Bulk elemental analysis data are compared from xray diffraction, xray fluorescence and fourier transform infrared spectroscopy. Hydrothermal synthesis and characterization of hydroxyapatite. Hydroxyapatite with uniform shape has been achieved using hydrothermal method. Eggshells a novel hydrothermal synthesis of nanohydroxyapatite from eggshellcalciumoxide precursors.
A hydrothermal method of synthesizing hydroxyapatite by heating a precipitate, formed by mixing cano 3 2 4h 2 o and nh 4 2 hpo 4 with distilled water, in a. The influence of ph and temperature on the morphology of. Calcium phosphates, calcium sulfate, hydroxyapatite, powder synthesis, hydrothermal synthesis. The effects of temperature on the hydrothermal synthesis of. Green synthesis and antibacterial activity of hydroxyapatite nanorods for orthopedic applications volume 7 issue 2 govindan suresh kumar, senkotuvel rajendran, sekar karthi, raji govindan, easwaradas kreedapathy girija, gopalu karunakaran, denis kuznetsov. Hydrothermal synthesis of hydroxyapatite from calcium pyrophosphate. Hydrothermal synthesis and nanostructure of carbonated calcium hydroxyapatite. The assynthesized samples were characterized by xray diffraction, fourier transform infrared spectroscopy, scanning electron microscopy, and. Hydrothermal synthesis of hydroxyapatite rods request pdf. Kandaswamya adepartment of biomedical engineering, psg college of technology, coimbatore 641004, tamil nadu, india. Hydroxyapatite is a bioceramic similar to the mineral component present in the human hard tissues and animal body. A hydrothermal method of synthesizing hydroxyapatite by heating a precipitate, formed by mixing cano 3 2 4h 2 o and nh 4 2 hpo 4 with distilled water, in a hydrothermal reactor at 200 o c for. Hydrothermal synthesis and biocompatibility study of highly crystalline carbonated hydroxyapatite nanorods caibao xue, yingzhi chen, yongzhuo huang, and peizhi zhu school of chemistry and chemical engineering, yangzhou university, jiangsu, 225009 china.
Both cuttlebone aragonite polymorph of caco 3 and caco 3 chemical calcite polymorph of caco 3 were used as caco 3 sources. Hydrothermal synthesis of hydroxyapatite nanopowders using. By controlling synthesis temperature and time, hydroxyapatite nanoparticles with welldefined sizes and morphology can be obtained. Ha can be synthesized using various methods including solid phase reaction method 12, precipitation, and hydrothermal 2. Hydrothermal synthesis of hydroxyapatite from calcium sulfate. Results showed that the rodlike nanohydroxyapatite changed its granule morphology into spherical. Hydrothermal synthesis of hydroxyapatite nanorods using a.
The effects of temperature on the hydrothermal synthesis. In this investigation, hydroxyapatite hap nanostructure with uniform morphologies, controllable size, nanodispersion and narrowsize distribution in diameter has been synthesized successfully by lowtemperature hydrothermal process, and the assynthesized powders were characterized by energydispersive xray spectroscopy, scanning electron microscopy, highresolution transmission electron. In the hydrothermal synthesis of various calcium phosphates, the precursor solution usually contains a calcium salt, a phosphate salt and a ph adjusting agent such as. Sem photographs of the surfaces of hydrothermally prepared magnetitehydroxyapatite ha composites with and without magnetite are shown in. Hydroxyapatite hap nanoparticles of tunable diameter were obtained by the precipitation method at room temperature and by microwave hydrothermal synthesis mhs. Hydrothermal, performed as a postsynthesis treatment, improves particle morphology, giving particles with regular surface contours, welldefined sizes and lower particle agglomeration. In this study, the effects of temperature on the hydrothermal synthesis of hydroxyapatitezeolite from blast furnace slag were investigated. The morphology of synthesized hap changed from small plateshaped to long needleshaped.
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