scholarly journals Gradual Replacement of Ca2+ with Mg2+ Ions in Brushite for the Production of Ca1−xMgxHPO4·nH2O Materials

Minerals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 284
Author(s):  
Mazen Alshaaer ◽  
Khalil Issa ◽  
Abdulaziz Alanazi ◽  
Saida Abu Mallouh ◽  
Ahmed S. Afify ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Calcium Nitrate ◽  
Ammonium Hydroxide ◽  
Magnesium Nitrate ◽  
Molar Ratio ◽  
Partial Replacement ◽  
Nitrate Hexahydrate ◽  
Calcium Nitrate Tetrahydrate ◽  
X Ray ◽  
Starting Solution

The present study investigates the gradual replacement of Ca2+ with Mg2+ ions in brushite (CaHPO4·2H2O). To date, this approach has not been systematically explored and may prove beneficial for the production of Ca1−xMgxHPO4·nH2O materials with tailored properties which are suitable for environmental and medical applications. For their production, solutions of sodium dihydrogen orthophosphate dehydrate, NaH2PO4·2H2O, calcium nitrate tetrahydrate, Ca(NO3)2·4H2O, magnesium nitrate hexahydrate, Mg(NO3)2·6H2O and ammonium hydroxide solution, NH4OH, were used. At low Mg/Ca molar ratios (up to 0.25) in the starting solution, partial replacement of Ca with Mg takes place (Mg doping) but no struvite is produced as discrete phase. When the Mg/Ca molar ratio increases gradually to 1.5, in addition to Mg-doped brushite, struvite, NH4MgPO4·6H2O, precipitates. The microstructure of the materials produced for different degrees of Ca replacement with Mg has been analyzed in depth with the use of powdered XRD (X-ray diffraction), XPS (X-ray photoelectron spectroscopy), thermogravimetric (TG) analysis and SEM (scanning electron microscopy). The results of this study prove that the Mg/Ca ratio in the starting solution can be monitored in such a way that materials with tailored composition are obtained.

Synthesis and characterization of pure and nanosized hydroxyapatite bioceramics

2017 ◽  
Vol 6 (2) ◽  
pp. 149-157 ◽  
Author(s):  
Aneela Anwar ◽  
Qudsia Kanwal ◽  
Samina Akbar ◽  
Aisha Munawar ◽  
Arjumand Durrani ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Calcium Nitrate ◽  
Temperature Stability ◽  
Molar Ratio ◽  
Calcium Nitrate Tetrahydrate ◽  
High Temperature Stability ◽  
X Ray ◽  
Transmission Electron ◽  
Nanosized Hydroxyapatite ◽  
Co Precipitation

AbstractSynthetic nanosized hydroxyapatite (HA) particles (<120 nm) were prepared using a co-precipitation technique by adopting two different routes – one from an aqueous solution of calcium nitrate tetrahydrate and diammonium hydrogen phosphate at pH 10 and the other by using calcium hydroxide and phosphoric acid as precursors at pH 8.5 and reaction temperature of 50°C. The lattice parameters of HA nanopowder were analogous to reference [Joint Committee on Powdered Diffraction Standards (JCPDS)] pattern no. 09-432. No decomposition of HA into other phases was observed even after heating at 1000°C in air for 1 h. This observation revealed the high-temperature stability of the HA nanopowder obtained using co-precipitation route. The effects of preliminary Ca/P molar ratio, precipitation, pH and temperature on the evolution of phase and crystallinity of the nanopowder were systematically examined and optimized. The product was evaluated by techniques such as X-ray-diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) and Raman spectroscopy analyses. The chemical structural analysis of the as-prepared HA sample was performed using X-ray photoelectron spectroscopy (XPS). After heat treatment at 1000°C for 1 h and ageing for 15 h, the product was obtained as a phase-pure, highly crystalline HA nanorods.

scholarly journals Effect of Ca2+ Replacement with Cu2+ Ions in Brushite on the Phase Composition and Crystal Structure

Minerals ◽  
2021 ◽  
Vol 11 (10) ◽  
pp. 1028
Author(s):  
Mazen Alshaaer ◽  
Juma’a Al-Kafawein ◽  
Ahmed S. Afify ◽  
Nagat Hamad ◽  
Ghassan Saffarini ◽  
...  
Keyword(s):  
Calcium Nitrate ◽  
Ammonium Hydroxide ◽  
Copper Nitrate ◽  
Molar Ratio ◽  
Calcium Nitrate Tetrahydrate ◽  
Molar Ratios ◽  
Starting Solution ◽  
Novel Approach ◽  
Nitrate Tetrahydrate ◽  
Microscopy Techniques

The gradual replacement of Ca2+ with Cu2+ ions in brushite (CaHPO4·2H2O) has been extensively studied and discussed. The approach adopted in this work has not been systematically explored in previous studies. This novel approach may prove beneficial for the production of Ca1−xCuxHPO4·nH2O materials with desired properties suitable for medical applications. Solutions of sodium dihydrogen orthophosphate dihydrate, NaH2PO4·2H2O, calcium nitrate tetrahydrate, Ca(NO3)2·4H2O, copper nitrate trihydrate, Cu(NO3)2·3H2O, ammonium hydroxide solution, and diluted HCl were used for the preparation of these materials. At low Cu/Ca molar ratios (up to 0.25) in the starting solution, biphasic phosphate minerals were formed: brushite and sampleite. When the Cu/Ca molar ratio increases gradually from 0.67 to 1.5, sampleite-like mineral precipitates. Powdered XRD (X-ray diffraction), thermogravimetric (TG) analysis, and SEM (scanning electron microscopy) techniques were employed for the study of the microstructure of the produced materials for different degrees of Ca replacement with Mg. It is found that the Cu/Ca ratio in the starting solution can be adjusted to obtain materials with tailored composition. Thus, a new method of sampleite-like synthesis as a rare mineral is introduced in this study. Both phosphate minerals brushite and sampleite-like minerals are attractive as precursors of bioceramics and biocements. The search for such products that may decrease the possibility of post prosthetic or implant infection can be crucial in preventing devastating post-surgical complications.

scholarly journals SEM, EDS, and XPS Characterization of Coatings Obtained on Titanium During AC Plasma Electrolytic Process Enriched in Magnesium

2018 ◽  
Vol 18 (3) ◽  
pp. 68-78 ◽  
Author(s):  
K. Rokosz ◽  
T. Hryniewicz ◽  
S. Raaen ◽  
D. Matýsek ◽  
Ł. Dudek ◽  
...  
Keyword(s):  
Calcium Nitrate ◽  
Zinc Nitrate ◽  
Magnesium Nitrate ◽  
Nitrate Hexahydrate ◽  
Calcium Nitrate Tetrahydrate ◽  
Porous Coatings ◽  
Magnesium Nitrate Hexahydrate ◽  
Xps Characterization ◽  
Micro Arc Oxidation ◽  
Plasma Electrolytic

AbstractPlasma Electrolytic Oxidation (PEO) known also as Micro Arc Oxidation (MAO) process is widely used to fabricate porous coatings on titanium and its alloys mainly in water- and acid-based solutions to different applications, e.g. in biomaterials, catalysts, and sensors. In the present paper, the SEM, EDS, and XPS results of porous coatings obtained by PEO treatment on titanium in electrolytes based on concentrated phosphoric H3PO4 acid with calcium nitrate tetrahydrate Ca(NO3)2·4H2O, or magnesium nitrate hexahydrate Mg(NO3)2·6H2O, or zinc nitrate hexahydrate Zn(NO3)2·6H2O for 3 minutes at 200 Vpp (peak to peak) with frequency of 50 Hz, are presented. Based on EDS results, the Ca/P, Mg/P, and Zn/P ratios, which equal to 0.95, 0.176, and 0.231, respectively, were found out. The XPS studies of the top 10 nm of the porous layer clearly indicate that it contains mainly phosphates (PO43− and/or HPO42− and/or H2PO4−, and/or P2O74−) with titanium (Ti4+) and calcium (Ca2+) or magnesium (Mg2+), or zinc (Zn2+).

scholarly journals Corrosive effects of nitrate-containing phase change materials used with copper

2016 ◽  
Vol 9 (2) ◽  
pp. 75-83 ◽  
Author(s):  
Vladimír Danielik ◽  
Peter Šoška ◽  
Katarína Felgerová
Keyword(s):  
Corrosion Rate ◽  
Phase Change ◽  
Phase Change Materials ◽  
Corrosion Behaviour ◽  
Calcium Nitrate ◽  
Magnesium Nitrate ◽  
Nitrate Hexahydrate ◽  
Calcium Nitrate Tetrahydrate ◽  
Magnesium Nitrate Hexahydrate ◽  
Nitrate Tetrahydrate

Abstract The paper presents the results of a study on the corrosion behaviour of copper (EN CW004A) in five possible phase change materials (PCMs): magnesium nitrate hexahydrate pure and with an addition of Mg(OH)2 (0.5 wt. %) or Sr(OH)2 (0.5 wt. %) at 90 °C, calcium nitrate tetrahydrate at 50 °C and a mixture of magnesium nitrate hexahydrate and calcium nitrate tetrahydrate (1:1 mass ratio) at 72 °C. The corrosion rate of copper samples is low except for the use of Mg(NO3)2 · 6H2O with/without an addition of Mg(OH)2. The lowest corrosion rate was observed for the mixture Mg(NO3)2 · 6H2O—Ca(NO3)2 · 4H2O (1:1), and it was ca six times lower than that of pure magnesium nitrate hexahydrate.

scholarly journals Novel Porous Phosphorus–Calcium–Magnesium Coatings on Titanium with Copper or Zinc Obtained by DC Plasma Electrolytic Oxidation: Fabrication and Characterization

Materials ◽  
2018 ◽  
Vol 11 (9) ◽  
pp. 1680 ◽  
Author(s):  
Krzysztof Rokosz ◽  
Tadeusz Hryniewicz ◽  
Sofia Gaiaschi ◽  
Patrick Chapon ◽  
Steinar Raaen ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Plasma Electrolytic Oxidation ◽  
Copper Ions ◽  
Calcium Nitrate ◽  
Porous Coating ◽  
Nitrate Hexahydrate ◽  
Calcium Nitrate Tetrahydrate ◽  
Porous Coatings ◽  
Electrolytic Oxidation ◽  
Plasma Electrolytic

In this paper, the characteristics of new porous coatings fabricated at three voltages in electrolytes based on H3PO4 with calcium nitrate tetrahydrate, magnesium nitrate hexahydrate, and copper(II) nitrate trihydrate are presented. The SEM, energy dispersive spectroscopy (EDS), glow discharge optical emission spectroscopy (GDOES), X-ray photoelectron spectroscopy (XPS), and XRD techniques for coating identification were used. It was found that the higher the plasma electrolytic oxidation (PEO) (micro arc oxidation (MAO)) voltage, the thicker the porous coating with higher amounts of built-in elements coming from the electrolyte and more amorphous phase with signals from crystalline Ca(H2PO4)2∙H2O and/or Ti(HPO4)2∙H2O. Additionally, the external parts of the obtained porous coatings formed on titanium consisted mainly of Ti4+, Ca2+, Mg2+ and PO43−, HPO42−, H2PO4−, P2O74− as well as Zn2+ or copper Cu+/Cu2+. The surface should be characterized by high biocompatibility, due to the presence of structures based on calcium and phosphates, and have bactericidal properties, due to the presence of zinc and copper ions. Furthermore, the addition of magnesium ions should accelerate the healing of postoperative wounds, which could lead to faster patient recovery.

scholarly journals Photocatalytic Reduction of CO2 to Methanol Using a Copper-Zirconia Imidazolate Framework

Catalysts ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 346
Author(s):  
Sonam Goyal ◽  
Maizatul Shima Shaharun ◽  
Ganaga Suriya Jayabal ◽  
Chong Fai Kait ◽  
Bawadi Abdullah ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Catalyst Support ◽  
Oxidation Potential ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Molar Ratios ◽  
Optimum Parameters ◽  
Reduction Of Co2 ◽  
Enhanced Yield

A set of novel photocatalysts, i.e., copper-zirconia imidazolate (CuZrIm) frameworks, were synthesized using different zirconia molar ratios (i.e., 0.5, 1, and 1.5 mmol). The photoreduction process of CO2 to methanol in a continuous-flow stirred photoreactor at pressure and temperature of 1 atm and 25 °C, respectively, was studied. The physicochemical properties of the synthesized catalysts were studied using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and photoluminescence (PL) spectroscopy. The highest methanol activity of 818.59 µmol/L.g was recorded when the CuZrIm1 catalyst with Cu/Zr/Im/NH4OH molar ratio of 2:1:4:2 (mmol/mmol/mmol/M) was employed. The enhanced yield is attributed to the presence of Cu2+ oxidation state and the uniformly dispersed active metals. The response surface methodology (RSM) was used to optimize the reaction parameters. The predicted results agreed well with the experimental ones with the correlation coefficient (R2) of 0.99. The optimization results showed that the highest methanol activity of 1054 µmol/L.g was recorded when the optimum parameters were employed, i.e., stirring rate (540 rpm), intensity of light (275 W/m2) and photocatalyst loading (1.3 g/L). The redox potential value for the CuZrIm1 shows that the reduction potential is −1.70 V and the oxidation potential is +1.28 V for the photoreduction of CO2 to methanol. The current work has established the potential utilization of the imidazolate framework as catalyst support for the photoreduction of CO2 to methanol.

Low-temperature route to nanoscale P3N5 hollow spheres

2003 ◽  
Vol 18 (10) ◽  
pp. 2359-2363 ◽  
Author(s):  
Hongzhou Gu ◽  
Yunle Gu ◽  
Zhefeng Li ◽  
Yongcheng Ying ◽  
Yitai Qian
Keyword(s):  
Photoelectron Spectroscopy ◽  
Hollow Spheres ◽  
Molar Ratio ◽  
Visible Absorption ◽  
X Ray ◽  
Transmission Electron ◽  
Influence Of Temperature On ◽  
Wide Gap ◽  
20 Nm ◽  
High Degree

Nanoscale hollow spheres of amorphous phosphorus nitride (P3N5) were synthesized by reacting PCl3 with NaN3 at 150–250 °C. Transmission electron microscope images show that the hollow spheres have a diameter of 150–350 nm, and the thickness of the shell is 20 nm. A very small amount of curly films were also found in the sample prepared at 150 °C. The infrared spectrum indicates a high degree of purity. X-ray photoelectron spectroscopy indicates the presence of P and N, with a molar ratio of 1:1.62 for P:N. Ultraviolet-visible absorption spectroscopy shows an absorption band at 265–315 nm. Under photoluminescent excitation at 230 nm, the P3N5 emits ultraviolet light at 305 nm. With a band gap of 4.28 eV, the products may be a wide gap semiconductor. A possible mechanism and the influence of temperature on the formation of the hollow spheres are also discussed.

scholarly journals Lead-Free BNT–BT0.08/CoFe2O4 Core–Shell Nanostructures with Potential Multifunctional Applications

Nanomaterials ◽  
2020 ◽  
Vol 10 (4) ◽  
pp. 672
Author(s):  
Marin Cernea ◽  
Roxana Radu ◽  
Harvey Amorín ◽  
Simona Gabriela Greculeasa ◽  
Bogdan Stefan Vasile ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Sol Gel ◽  
Molar Ratio ◽  
Transmission Electron Microscopy Data ◽  
Core Shell ◽  
Shell Nanoparticles ◽  
Two Phase ◽  
X Ray ◽  
Shell Nanostructures

Herein we report on novel multiferroic core–shell nanostructures of cobalt ferrite (CoFe2O4)–bismuth, sodium titanate doped with barium titanate (BNT–BT0.08), prepared by a two–step wet chemical procedure, using the sol–gel technique. The fraction of CoFe2O4 was varied from 1:0.5 to 1:1.5 = BNT–BT0.08/CoFe2O4 (molar ratio). X–ray diffraction confirmed the presence of both the spinel CoFe2O4 and the perovskite Bi0.5Na0.5TiO3 phases. Scanning electron microscopy analysis indicated that the diameter of the core–shell nanoparticles was between 15 and 40 nm. Transmission electron microscopy data showed two–phase composite nanostructures consisting of a BNT–BT0.08 core surrounded by a CoFe2O4 shell with an average thickness of 4–7 nm. Cole-Cole plots reveal the presence of grains and grain boundary effects in the BNT–BT0.08/CoFe2O4 composite. Moreover, the values of the dc conductivity were found to increase with the amount of CoFe2O4 semiconductive phase. Both X-ray photoelectron spectroscopy (XPS) and Mössbauer measurements have shown no change in the valence of the Fe3+, Co2+, Bi3+ and Ti4+ cations. This study provides a detailed insight into the magnetoelectric coupling of the multiferroic BNT–BT0.08/CoFe2O4 core–shell composite potentially suitable for magnetoelectric applications.

scholarly journals Photoreduction of Carbon Dioxide to Methanol over Copper Based Zeolitic Imidazolate Framework-8: A New Generation Photocatalyst

Catalysts ◽  
2018 ◽  
Vol 8 (12) ◽  
pp. 581 ◽  
Author(s):  
Sonam Goyal ◽  
Maizatul Shaharun ◽  
Chong Kait ◽  
Bawadi Abdullah ◽  
Mariam Ameen
Keyword(s):  
Photocatalytic Activity ◽  
Photoelectron Spectroscopy ◽  
Ammonium Hydroxide ◽  
Photocatalytic Reduction ◽  
Zeolitic Imidazolate Framework ◽  
X Ray ◽  
Efficient Reduction ◽  
Vis Spectroscopy ◽  
Metal Organic ◽  
Reduction Of Co2

The efficient reduction of CO2 into valuable products such as methanol, over metal-organic frameworks (MOFs) based catalyst, has received much attention. The photocatalytic reduction is considered the most economical method due to the utilization of solar energy. In this study, Copper (II)/Zeolitic Imidazolate Framework-8 (Cu/ZIF-8) catalysts were synthesized via a hydrothermal method for photocatalytic reduction of CO2 to methanol. The synthesized catalysts were characterized by X-ray Photoelectron Spectroscopy (XPS), Field Emission Scanning Electron Microscopy (FESEM) coupled with Energy Dispersive X-ray (EDX), Ultraviolet-visible (UV-vis) spectroscopy, and X-Ray Diffraction (XRD). The host ZIF-8, treated with 2 mmol copper prepared in 2M ammonium hydroxide solution showed the highest photocatalytic activity. The crystal structures of ZIF-8 and 2Cu/ZIF-8N2 catalysts were observed as cubic and orthorhombic, respectively and the XPS analysis confirmed the deposition of Cu (II) ions over ZIF-8 surface among all the prepared catalysts. The orthorhombic structure, nano-sized crystals, morphology and Cu loading of the 2Cu/ZIF-8N2 catalyst were the core factors to influence the photocatalytic activity. The yield of Methanol was found to be 35.82 µmol/L·g after 6 h of irradiations on 2Cu/ZIF-8N2 catalyst in the wavelength range between 530–580 nm. The copper-based ZIF-8 catalyst has proven as an alternative approach for the economical photocatalytic reduction of CO2 to CH3OH.

Sign in / Sign up

Export Citation Format

Share Document