scholarly journals Hydrogen-substituted β-tricalcium phosphate synthesized in organic media

Author(s):  
Christoph Stähli ◽  
Jürg Thüring ◽  
Laëtitia Galea ◽  
Solène Tadier ◽  
Marc Bohner ◽  
...  

β-Tricalcium phosphate (β-TCP) platelets synthesized in ethylene glycol offer interesting geometries for nano-structured composite bone substitutes but were never crystallographically analyzed. In this study, powder X-ray diffraction and Rietveld refinement revealed a discrepancy between the platelet structure and the known β-TCP crystal model. In contrast, a model featuring partial H for Ca substitution and the inversion of P1O4tetrahedra, adopted from the whitlockite structure, allowed for a refinement with minimal misfits and was corroborated by HPO42−absorptions in Fourier-transform IR spectra. The Ca/P ratio converged to 1.443 ± 0.003 (n= 36), independently of synthesis conditions. As a quantitative verification, the platelets were thermally decomposed into hydrogen-free β-TCP and β-calcium pyrophosphate which resulted in a global Ca/P ratio in close agreement with the initial β-TCP Ca/P ratio (ΔCa/P = 0.003) and with the chemical composition measured by inductively coupled plasma (ΔCa/P = 0.003). These findings thus describe for the first time a hydrogen-substituted β-TCP structure,i.e.a Mg-free whitlockite, represented by the formula Ca21 − x(HPO4)2x(PO4)14 − 2x, wherex= 0.80 ± 0.04, and may have implications for resorption properties of bone regenerative materials.

2020 ◽  
Vol 10 (6) ◽  
pp. 6837-6845

β-tricalcium phosphate (β-TCP) is a bioceramic with unique osteoinductive and osteoconductive properties. It can be obtained by calcining calcium-deficient apatites (CDHA) at 750°C and above. The reduction of calcining temperature or the stabilization of the β phase, by doping, is therefore of particular interest. This paper investigates the preparation of CDHA with a theoretical 0.05 Mg/(Ca + Mg) ratio and (Ca+Mg)/P = 1.55 via precipitation method, and the resultant powder is calcined at a different temperature ranging from 80 to 715°C. The as-synthesized undoped powder was used as the reference in this study. The effect of calcination temperature and composition were investigated by the aid of X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), inductively coupled plasma optical emission spectroscopy (ICP-OES) and scanning electron microscopy (SEM). The study indicated that the powder was pure Mg-doped beta-tricalcium phosphate. The incorporation of Mg within the calcium phosphate lattice promoted the formation and stabilization of the β -TCP phase at a lower temperature.


Molecules ◽  
2021 ◽  
Vol 26 (5) ◽  
pp. 1462
Author(s):  
Hao Xu ◽  
Jie Zhu ◽  
Xiong Wang ◽  
Chao Shen ◽  
Shengshen Meng ◽  
...  

Developing sustainable routes for the synthesis of zeolites is still a vital and challenging task in zeolite scientific community. One of the typical examples is sustainable synthesis of aluminosilicate EU-1 zeolite, which is not very efficient and environmental-unfriendly under hydrothermal condition due to the use of a large amount of water as solvent. Herein, we report a sustainable synthesis route for aluminosilicate EU-1 zeolite without the use of solvent for the first time. The physicochemical properties of the obtained EU-1 zeolite are characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetry-differential thermal analysis (TG-DTA), N2 sorption, inductively coupled plasma (ICP) analysis, and solid nuclear magnetic resonance (NMR), which show the product has high crystallinity, uniform morphology, large BET surface area, and four-coordinated aluminum species. Moreover, the impact of synthesis conditions is investigated in detail. The sustainable synthesis of aluminosilicate EU-1 zeolite under solvent-free


2020 ◽  
Vol 9 (1) ◽  
pp. 1586-1593
Author(s):  
Tingting Yan ◽  
Shengwen Zhong ◽  
Miaomiao Zhou ◽  
Xiaoming Guo ◽  
Jingwei Hu ◽  
...  

Abstract The extraction of Li from the spent LiFePO4 cathode is enhanced by the selective removal using interactions between HCl and NaClO to dissolve the Li+ ion while Fe and P are retained in the structure. Several parameters, including the effects of dosage and drop acceleration of HCl and NaClO, reaction time, reaction temperature, and solid–liquid ratio on lithium leaching, were tested. The Total yields of lithium can achieve 97% after extraction process that lithium is extracted from the precipitated mother liquor, using an appropriate extraction agent that is a mixture of P507 and TBP and NF. The method also significantly reduced the use of acid and alkali, and the economic benefit of recycling is improved. Changes in composition, morphology, and structure of the material in the dissolution process are characterized by inductively coupled plasma optical emission spectrometry, scanning electron microscope, X-ray diffraction, particle size distribution instrument, and moisture analysis.


2006 ◽  
Vol 118 ◽  
pp. 639-644
Author(s):  
Hye Sung Kim ◽  
Su Chak Ryu

Hydroxyapatite (Ca10(PO4)6(OH)2, HAp) powders is synthesized using the mixed powders of CaCO3 refined from oyster shells and phosphoric acid (H3PO4-98%, Daejung) as starting materials. The characteristic evaluation and chemical analysis of the synthesized powders is performed by X-ray diffraction (XRD), Fourier-transformed infra-red spectroscopy (FT-IR), and inductively-coupled plasma atomic emission spectroscopy (ICPAES). XRD analysis of synthetic powder by heat treatment at 1300°C for 2hrs shows only HAp peaks corresponding to stoichiometric HAp. It is confirmed by ICP-AES test that impurities such as Zn, In, Ti, Ba, Cd, Pb, and Mn, is not detected at all, but small amounts of Ti and Be is observed (0.099ppm Ti and 0.002ppm Ba). Variation of bone density is measured by giving medication of HAp powder with drinking water into human body continuously for three month. After the medication, the bone density is higher than the medication before. This means that HAp powder made from this process can be used as improver of bone density.


2012 ◽  
Vol 9 (4) ◽  
pp. 1788-1795 ◽  
Author(s):  
Olushola S. Ayanda ◽  
Olalekan S. Fatoki ◽  
Folahan A. Adekola ◽  
Bhekumusa J. Ximba

In this study, fly ash was obtained from Matla power station and the physicochemical properties investigated. The fly ash was characterized by x-ray fluorescence, x-ray diffraction, scanning electron microscopy, and inductively coupled plasma mass spectrometry. Surface area, particle size, ash and carbon contents, pH, and point of zero charge were also measured. The results showed that the fly ash is alkaline and consists mainly of mullite (Al6Si2O13) and quartz (SiO2). Highly toxic metals As, Sb, Cd, Cr, and Pb as well as metals that are essential to health in trace amounts were also present. The storage and disposal of coal fly ash can thus lead to the release of leached metals into soils, surface and ground waters, find way into the ecological systems and then cause harmful effect to man and its environments.


Author(s):  
Shiying Zhang ◽  
Lei Zhang ◽  
Yueyao Zhong ◽  
Guodong Wang ◽  
Qingjun Xu

High crystal quality GaN nanorod arrays were fabricated by inductively coupled plasma (ICP) etching using self-organized nickel (Ni) nano-islands mask on GaN film and subsequent repaired process including annealing in ammonia and KOH etching. The Ni nano-islands have been formed by rapid thermal annealing, whose density, shape, and dimensions were regulated by annealing temperature and Ni layer thickness. The structural and optical properties of the nanorods obtained from GaN epitaxial layers were comparatively studied by high-resolution X-ray diffraction (HRXRD), Raman spectroscopy and photoluminescence (PL). The results indicate that damage induced by plasma can be successfully healed by annealing in NH3 at 900 °C. The average diameter of the as-etched nanorod was effectively reduced and the plasma etch damage was removed after a wet treatment process in a KOH solution. It was found that the diameter of the GaN nanorod was continuously reduced and the PL intensity first increased, then reduced and finally increased as the KOH etching time sequentially increased.


2018 ◽  
Vol 56 ◽  
pp. 23-33
Author(s):  
Mar Rey-Solé ◽  
Maria Pilar García-Argüelles ◽  
Jordi Nadal ◽  
Xavier Mangado ◽  
Anders Scherstén ◽  
...  

The l’Hort de la Boquera site is located in the northeastern part of Iberia and its stone tool assemblage includes up to 25,000 flint artefacts. This is the first approach to the analysis of the raw material through an archaeopetrological study. Results were obtained by use of mineralogi¬cal techniques: macroscopic and petrographic analysis, Scanning Electronic Microscopy (SEM), Micro-Raman and X-Ray diffraction (XRD); additionally, Laser Ablation Inductively Coupled Plasma Mass Spectrometry was applied. It has been possible to discriminate at least four flint categories, the ‘Evaporitic flint type’ (with two local subvarieties – ‘Common evaporitic’ and ‘Garnet’ varieties) that comes from local outcrops of the Ulldemolins Complex, and two flint types that had their origin further afield: the ‘Charophyta flint type’ (coming from the Torrente de Cinca Unit) and the ‘Dark flint type’ (from the La Serra Llarga Formation).These results make this study the most comprehensive analysis of raw materials that has been carried out in the area so far


2006 ◽  
Vol 71 (11) ◽  
pp. 1153-1160 ◽  
Author(s):  
Chang Hu-Yuan ◽  
Feng Li ◽  
Li. Hua ◽  
Bin Zhang

As prepared carbon nanotubes were pretreated with nitric acid (CNTs-HNO3) or ammonia (CNTs-NH3). Fourier transform infrared spectroscopy (FTIR) measurements showed that the surface of the nanotubes was functionalized with carboxylic and hydroxyl functional groups after the acid treatment and that basic groups containing nitrogen, such as N-H and C-N, were introduced to the surface of the nanotubes after the ammonia treatment. X-Ray diffraction analysis implied that the nickel residue in the CNTs was effectively removed by acid treatment. However, the nickel residue was only partially eliminated by ammonia pretreatment. NiB amorphous catalysts supported on CNTs-HNO3 and CNTs-NH3 were prepared by the impregnation-chemical reduction method and characterized by transmission electron microscopy (TEM), as well as inductively coupled plasma (ICP) spectroscopy and studied in the selective hydrogenation of acetylene. TEM measurements showed that a high density NiB particles of about 9 nm were homogeneously dispersed on the CNTs-NH3. However, NiB particles (13-23 nm)with amean size of 16 nm were scattered on the CNTs-HNO3.As a result, the activity and selectivity of NiB/CNTs-NH3 were higher than those of NiB/CNTs-HNO3 in the selective hydrogenation of acetylene.


Author(s):  
Nitu Bhatnagar ◽  
Avani Pareek

The present study is aimed to observe the difference in the Physico-Chemical characteristics of the marketed and formulated bhasma samples through X-Ray Diffraction analysis (XRD), Dynamic Light Scattering (DLS), Zeta potential, Thermo-Gravimetric analysis (TGA), Scanning Electron Microscopy (SEM) and Energy Dispersive X-Ray analysis (EDAX), apart from organoleptic methods. Inductively Coupled Plasma Mass Spectroscopy (ICPMS) analysis was also done to observe the presence of trace and heavy metals so that the safety of all these samples could be ensured. XRD shows variation in oxide nature of zinc as well crystallite size in all bhasma samples. DLS and SEM results show difference in particle size of marketed bhasma samples as compared to formulated Yashada bhasma. EDAX and ICPMS also confirm the alteration in elemental composition of all these bhasma samples. Thus, it can be concluded that these ayurvedic medicines should be prepared strictly using the formulation methods as mentioned in the Ayurvedic texts. This will help the prepared products to adopt the inherent quality of the ancient system of medicine, which shall be useful and devoid of any side effects for human consumption.


Minerals ◽  
2019 ◽  
Vol 9 (7) ◽  
pp. 402 ◽  
Author(s):  
Qin ◽  
Cao ◽  
Wei ◽  
Wang ◽  
Liu

This paper reports the mineral compositions and geochemical characteristics of the No. 5-2 high-sulfur coal (Taiyuan Formation) from Dongpo Mine, Weibei Coalfield, Shaanxi, Northern China via transmitted and reflected light microscopy, scanning electron microscope equipped with an energy-dispersive X-ray spectrometer (SEM-EDS), X-ray diffraction (XRD), inductively coupled plasma mass spectrometry (ICP-MS), and X-ray fluorescence spectrometry (XRF). We also confirmed the input of intermediate-felsic volcanic ashes into the Taiyuan Formation coals in Dongpo Mine, Weibei Coalfield. The results show that Dongpo coals are enriched in Ga and Li compared to the average values for world hard coals, and they are depleted in Al2O3 compared to Chinese coals. The coal low temperature ash contains kaolinite, illite, quartz, calcite, pyrite, and to a lesser extent, chlorite, plagioclase, dolomite, ankerite, and apatite. The concentration anomalies of Ga and Li in No. 5-2 high-sulfur coal were not caused by the Benxi Formation Bauxite, but by the influence of multiple geological factors. The Middle Proterozoic moyite from the Yinshan Oldland led to the slightly higher Ga and Li contents of the No. 5-2 coal than those in world hard coals. Input of synchronization volcanic ash, injection of hydrothermal fluids during the syngenetic or early diagenetic stages and influence of seawater further contributed to the Ga and Li enrichment of the No. 5-2 coal.


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