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

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.

From 1D to 2D Cd(II) and Zn(II) Coordination Networks by Replacing Monocarboxylate with Dicarboxylates in Partnership with Azine Ligands: Synthesis, Crystal Structures, Inclusion, and Emission Properties

Eight mixed-ligand coordination networks, [Cd(2-aba)(NO3)(4-bphz)3/2]n·n(dmf) (1), [Cd(2-aba)2(4-bphz)]n·0.75n(dmf) (2), [Cd(seb)(4-bphz)]n·n(H2O) (3), [Cd(seb)(4-bpmhz)]n·n(H2O) (4), [Cd(hpa)(3-bphz)]n (5), [Zn(1,3-bdc)(3-bpmhz)]n·n(MeOH) (6), [Cd(1,3-bdc)(3-bpmhz)]n ·0.5n(H2O)·0.5n(EtOH) (7), and [Cd(NO3)2(3-bphz)(bpe)]n·n(3-bphz) (8) were obtained by interplay of cadmium nitrate tetrahydrate or zinc nitrate hexahydrate with 2-aminobenzenecarboxylic acid (H(2-aba)), three dicarboxylic acids, sebacic (decanedioic acid, H2seb), homophthalic (2-(carboxymethyl)benzoic acid, H2hpa), isophthalic (1,3-benzenedicarboxylic acid, H2(1,3-bdc)) acids, bis(4-pyridyl)ethane (bpe) and with four azine ligands, 1,2-bis(pyridin-4-ylmethylene)hydrazine (4-bphz), 1,2-bis(1-(pyridin-4-yl)ethylidene) hydrazine (4-bpmhz), 1,2-bis(pyridin-3-ylmethylene)hydrazine (3-bphz), and 1,2-bis(1-(pyridin-3-yl) ethylidene)hydrazine (3-bpmhz). Compounds 1 and 2 are 1D coordination polymers, while compounds 3–8 are 2D coordination polymers. All compounds were characterized by spectroscopic and X-ray diffraction methods of analysis. The solvent uptakes and stabilities to the guest evacuation were studied and compared for 1D and 2D coordination networks. The de-solvated forms revealed a significant increase of emission in comparison with the as-synthesized crystals.

Biofilms of cellulose and hydroxyapatite composites: Alternative synthesis process

A new biofilm of cellulose coated with hydroxyapatite particles have been prepared using a simple, fast and low temperature process based on a microwave-assisted hydrothermal synthesis. The cellulose used as matrix of the biocomposite was extracted from banana stems residues. The hydroxyapatite coating was performed using calcium nitrate tetrahydrate, phosphoric acid, and 1,2-ethylenediamine dispersed in a cellulose/water solution, with posterior microwave-assisted hydrothermal synthesis, for 5 min at 140°C. The chemical, structural, thermal, and morphological properties of the composites were investigated by X-ray diffraction, infrared spectroscopy, thermogravimetry and field emission scanning electron microscopy. Results showed that the methodology was effective to produce high quality composites, with good thermal stability. Cell viability tests indicated that the cellulose/Hap films were not cytotoxic.

Synthesis of Graphene Nanoribbons–Hydroxyapatite Nanocomposite Applicable in Biomedicine and Theranostics

In order to investigate the effect of graphene nanoribbons on the final properties of hydroxyapatite-based nanocomposites, a solvothermal method was used at 180 °C and 5 h for the synthesis of graphene nanoribbons–hydroxyapatite nanopowders by employing hydrogen gas injection. Calcium nitrate tetrahydrate and diammonium hydrogenphosphate were used as calcium and phosphate precursors, respectively. To synthesize the powders, a solvent containing diethylene glycol, anhydrous ethanol, dimethylformamide, and water was used. Graphene oxide nanoribbons were synthesized by chemical unzipping of carbon nanotubes under oxidative conditions. The synthesized powders were consolidated by spark plasma sintering methodat 950 °C and a pressure of 50 MPa. The powders and sintered samples were then evaluated using X-ray diffraction, Raman spectroscopy, high-resolution transmission electron microscopy, Vickers microindentation techniques, and biocompatibility assay. The findings of this study showed that the final powders synthesized by the solvothermal method had calcium to phosphate ratio of about 1.67. By adding a small amount of graphene nanoribbon (0.5%W), elastic modulus and hardness of hydroxyapatite increased dramatically. In biological experiments, the difference of hydroxyapatite effect in comparison with the nanocomposite was not significant. The findings of this study showed that graphene nanoribbons have a positive effect on the properties of hydroxyapatite, and these findings would be useful for the medical and theranostic application of this type of nanocomposites.

Synthesis of plate-like β-tricalcium phosphate nanoparticles and their efficiency in remineralization of incipient enamel caries

The purpose of this study was to synthesize nano-sized β-tricalcium phosphate (nano-TCP) particles and determine its concentration-dependent properties on incipient enamel caries lesions. Nano-TCP was synthesized as a wet chemical through a method using low concentration of precursors and low addition rate of calcium nitrate tetrahydrate as a second phase. Morphology and phase composition of the particles were analyzed by SEM, XRD, and EDXA techniques. Incipient enamel lesions were created in human premolars with an acidic buffer. The teeth were then incubated in aqueous dispersions of nano-TCP as remineralization solutions. Sodium fluoride solution and deionized water were used as positive and negative control groups, respectively. The quality and thickness of the remineralized layer on enamel were investigated using SEM. The data were statistically analyzed by analysis of variance (ANOVA) and post hoc Tukey’s test. The synthesized nano-TCP mostly consisted of porous platelet-like crystals of 50–100 nm thickness and pore diameters of 100–300 nm. SEM observation showed that a homogenous layer was formed on the surface of the enamels remineralized in nano-TCP solutions. The thickness of the mineralized layer was dependent on the incubation time and nano-TCP concentration.

Low temperature synthesis of wollastonite using sol–gel combustion method: In vitro bioactivity evaluation

In this paper, low temperature, economical sol–gel combustion method was adopted to synthesize wollastonite ceramic. Calcium nitrate tetrahydrate and tetraethyl orthosilicate were taken as source for Ca and Si, while citric acid and nitric acid were used as chelating/combustion agents. The yielded powder calcined at 600[Formula: see text]C for 4 h was characterized by FTIR, XRD and SEM techniques. Results showed that the citrate combustion method was the most efficient method to prepare wollastonite at low temperature. Moreover, in vitro bioactivity test performed in simulated body fluid (SBF) showed good bioactivity of synthesized wollastonite ceramics.

Pengaruh Konsentrasi Larutan Prekursor Terhadap Morfologi dan Ukuran Kristal Nanopartikel Seng Oksida

Pengaruh konsentrasi larutan prekursor terhadap morfologi dan ukuran nanopartikel seng oksida (ZnO) yang disintesis menggunakan metode hidrotermal telah diteliti. Larutan ZnO dengan konsentrasi 15 mM, 20 mM, 25 mM, 30 mM dan 35 mM disiapkan menggunakan prekursor zinc nitrate tetrahydrate dan hexamethylenetetramine dengan pelarut aquades. Morfologi nanopartikel ZnO yang terbentuk dikarakterisasi menggunakan Scanning Electron Microscope (SEM) dan ukuran kristal dikarakterisasi menggunakan XRD. Hasil karakterisasi menggunakan SEM menujukkan bahwa sampel yang tebentuk mengalami aglomerasi. Hasil karakterisasi XRD menunjukkan bahwa sampel adalah ZnO dengan struktur heksagonal Ukuran kristal dihitung menggunakan persamaan Debye-Scherrer dan diperoleh bahwa ukuran kristal berada pada rentang 25,4 – 27,5 nm. Dari penelitian diperoleh bahwa variasi konsentrasi larutan prekursor menyebabkan adanya perubahan ukuran kristal tapi tidak terlalu signifikan.Kata kunci: Zno, hidrotermal, ukuran kristal

An unsymmetrical dinuclear scandium complex comprising salophen ligands [H2salophen = N,N′-bis(salicylidene)-1,2-phenylenediamine]

Treatment of scandium nitrate tetrahydrate with the tetradentate ligand H2salophen [N,N′-bis(salicylidene)-1,2-phenylenediamine] afforded the yellow dinuclear complex Sc(NO3)2(μ-salophen)Sc(salophen)(EtOH) or [Sc2(C20H14N2O2)2(NO3)2(C2H6O)] (systematic name: (ethanol-κO)bis(nitrato-κ2 O,O′){μ-2,2′-[1,2-phenylenebis(nitrilomethanylylidene)]diphenolato-κ4 N,N′,O,O′:κ2 O,O′}{2,2′-[1,2-phenylenebis(nitrilomethanylylidene)]diphenolato-κ4 O,N,N′,O′}discandium). In this compound, one salophen ligand displays a bridging coordination via the two oxygen atoms, while the other salophen ligand is attached to only one Sc center. This arrangement is stabilized by a hydrogen-bonded EtOH co-ligand, and by π–π stacking interactions between the two salophen ligands.

Manganese Fluorene Phosphonates: Formation of Isolated Chains

9,9-dimethylfluorenyl-2-phosphonic acid 1 was reacted with manganese nitrate tetrahydrate to produce under hydrothermal conditions the crystalline manganese phosphonate Mn(H2O)2[O2(OH)PC15H13]2·2H2O which crystallize in the P21/c space group. This compound is a rare example of Mn-phosphonate material featuring isolated chains. The interactions between these chains containing the 9,9-dimethylfluorenyl moieties, result from Van der Waals interactions involving the fluorene ligands and C···H–C hydrogen bonds as revealed by Hirshfeld Surfaces. This material features antiferromagnetic exchange interactions as revealed by the magnetic susceptibility as a function of the temperature.