N-Lauroyl sarcosine sodium salt mediated formation of hydroxyapatite microspheres via a hydrothermal route

Dandelion-like hydroxyapatite (HA) microspheres were successfully prepared using Ca(NO₃)₂·4H₂O and (NH₄)₃PO₄·3H₂O as raw materials and N-Lauroyl sarcosine sodium salt (Sar-Na) as template via a hydrothermal route. The chemical composition, structure, morphology and thermal properties of the samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscope (FTIR), Scanning electron microscope (SEM) and Thermal gravimetric analysis (TG), respectively. The results demonstrate that, Sar-Na has great impact on the morphology of HA. With increasing the amount of Sar-Na, the morphology of HA varies from nanograins to nanorods, finally grows into dandelion-like microstructure. The obtained dandelion-like HA microspheres about 6 μm in diameter are composed of radially oriented nanorods. Furthermore, the possible formation mechanism of morphology change is also discussed.     

Electrospun hydroxyapatite fibers from a simple sol-gel system

This work reports the production of hydroxyapatite (HA) sub-micron fibers by combining electrospinning and a non-alkoxide sol-gel system, using cheap precursors. Phosphorus pentoxide (P₂O₅) and calcium nitrate tetrahydrate (Ca(NO₃)₂.4H₂O) were used as precursors of phosphorus and calcium, respectively. The fibers were electrospun from a mixture of the gel formed from the system Ca(NO₃)₂.4H₂O/P₂O₅ with polymeric solutions of polyvinylpyrrolidone (PVP) in water and ethanol/water mixtures. The fibers were analyzed for their morphology (Scanning Electron Microscopy, SEM), chemical composition (Fourier Transform Infrared Spectroscopy, FTIR) and structure (X-ray diffraction, XRD). The fibers obtained were composed mainly of type B carbonated HA with traces of β-tricalcium phosphate (β-TCP). SEM analysis revealed that increasing the concentration of water in the solvent system, used in the preparation of electrospinning solutions, led to fibers with smaller diameters and narrower diameter distribution.     

Synthesis and properties of calcium hydroxyapatite/silk fibroin organomineral composites

The coprecipitation of calcium hydroxyapatite (HA) (Ca₁₀(PO₄)₆(OH)₃) and silk fibroin (SF) from an aqueous solution in the Ca(NO₃)₂–(NH₄)₂HPO₄–NH₃–H₂O–SF system has been used to synthesize HA/SF organomineral composites based on nanocrystalline HA, containing 2, 5, and 10 wt % SF. The synthesis products were characterized by X-ray diffraction, thermogravimetric analysis, infrared spectroscopy, scanning electron microscopy, and electron spectroscopy for chemical analysis.     

Hydroxyapatite nanospindles by biomimetic synthesis with chitosan as template

Abstract

Based on the principles of biomineralisation, spindle shaped hydroxyapatites (HA) were synthesised through the biomimetic method with chitosan (CS) as template. The microstructure, chemical composition and thermal behaviour were characterised by means of X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and thermogravimetry differential thermal analysis (TGDTA) respectively. The results show that the spindle shaped nanoHA, 30–40 nm in length and 7–8 nm in width, were synthesised with 0·5 wt-%CS as template in 6% (v/v) hydrogen peroxide solution for 7 days. The crystallinity of samples increased with the aging time. TGDTA analyses show that the HA powders synthesised with CS as template contain CS molecules and have good thermal stability up to 800°C.     

Polymer-assisted synthesis of hydroxyapatite nanoparticle

Hydroxyapatite (HA, Ca₁₀(PO₄)₆(OH)₂) nanoparticles were synthesized using calcining calcium dihydrogenphosphate (Ca(H₂PO₄)₂ · H₂O), calcium hydroxide (Ca(OH)₂), and polyethylene glycol (PEG) at 900 °C in an oxygen atmosphere. This one-step process yields HA nanoparticles with similar particle sizes (e.g., 50–80 nm) that are well-crystallized and non-aggregated. PEG is an important factor in controlling the particle size, crystal phase, and degree of aggregation in these HA particles. This conclusion is supported by results from a field-emission scanning electron microscope (FE-SEM), X-ray diffractometry (XRD), energy dispersive X-ray analysis (EDS), a high-resolution transmission electron microscope (HR-TEM), and dynamic light scattering (DLS).     

Controlled synthesis of gold nanosnakes assisted by poly(vinyl pyrrolidone)–sodium dodecyl sulphate aggregations

Anisotropic single-crystalline gold nanosnakes were synthesised in poly(vinyl pyrrolidone) (PVP)–sodium dodecyl sulphate (SDS) aggregation aqueous solution by reducing HAuCl₄ with PVP without any additional reducing agent. The crystal structures, growth process and the influence of SDS concentrations on the growth of gold nanosnakes have been investigated by X-ray diffraction and transmittance electron microscopy. In this approach, the peculiar structure of PVP–SDS aggregations is indispensable for the asymmetrical formation of gold nanosnakes. Without PVP–SDS aggregations, only long tortuous gold nanobelts were synthesised. When SDS concentration was increased from 3 to 10?mM, gold nanosnakes, nanokites and nanoplates were fabricated. To the best of our knowledge, this is the first report on the SDS-induced shape transformation from snake-like to plate-like at fixed low HAuCl₄ concentration in PVP–SDS aggregation aqueous solutions. Moreover, the gold nanosnakes exhibit excellent electrocatalytic property towards the oxidation of methanol indicating their potential applications in fuel cells, catalysis, biosensing and nanodevices.     

Preparation and electrochemical performances of LiFePO4/C composite nanobelts via facile electrospinning

LiFePO₄/C composite nanobelts were synthesized by calcination of the [LiOH + Fe(NO₃)₃ + H₃PO₄]/polyvinyl pyrrolidone (PVP) electrospun nanobelts. PVP was used as the electrospinning template and carbon source. During the calcination, [LiOH + Fe(NO₃)₃ + H₃PO₄] were transformed to lithium iron phosphate (LiFePO₄) and PVP was decomposed into carbon. The morphology and properties of the as-prepared samples were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Brunauer–Emmett–Teller (BET) specific surface area analysis, electrochemical impedance spectroscopy and galvanostatic charge–discharge measurements. The results indicate that the mean width of LiFePO₄/C composite nanobelts is 2.50 ± 0.33 μm, the average thickness is about 162 nm and the BET specific surface area is 19.4 m² g^?1. The addition of carbon does not affect the structure of LiFePO₄, but improves its electrochemical performances. At the current density of 0.2 C, the initial discharge capacity of LiFePO₄/C electrode is 123.38 mAh g^?1 and there is no obvious capacity fading after 50 cycles. The formation mechanism of LiFePO₄/C composite nanobelts was also proposed.     

Electrospinning fabrication and electrochemical properties of LiFePO4/C composite nanofibers

LiFePO₄/C composite nanofibers were synthesized by calcination of the [LiOH + Fe(NO₃)₃ + H₃PO₄]/PVP electrospun nanofibers. Polyvinyl pyrrolidone (PVP) was used as the electrospinning template and carbon source. During the calcination [LiOH + Fe(NO₃)₃ + H₃PO₄] were transformed to LiFePO₄ and PVP was decomposed into carbon. The morphology and properties of the as-prepared samples were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Brunauer–Emmett–Teller (BET) specific surface area analysis, electrochemical impedance spectroscopy and galvanostatic charge–discharge measurements. The results indicate that the mean diameter of as-prepared LiFePO₄/C composite nanofibers is 179.08 ± 29.66 nm and the BET specific surface area is 66.59 m² g^?1. The addition of carbon does not affect the structure of LiFePO₄, but improves its electrochemical performances. At the current density of 0.2 C, the initial discharge capacity of LiFePO₄/C electrode is 133.6 mAh g^?1 and there is no obvious capacity fading after 100 cycles. The formation mechanism of the LiFePO₄/C composite nanofibers was also proposed.     

Synthesis of gold nanoparticles of variable morphologies using aqueous leaf extracts of Cocculus hirsutus

Spherical, triangular (prismatic) and square plate shaped gold nanoparticles have been synthesised from HAuCl₄?·?3H₂O solution using the aqueous leaf extract of Cocculus hirsutus. Nanoparticles are characterised using higher resolution transmission electron microscope, X-ray diffraction and UV–Vis absorption spectroscopic study. FT-IR analysis reveals that the gold nanostructures are mostly stabilised by the carbonyl and amide groups present in the active component of C. hirsutus leaf extract. Formation of gold nanostructures of variable morphologies has been explained due to slow reduction of gold ions by the mild reducing ascorbic acid present within the extract and this controlled reduction assists the preferential deposition of Au atom on different lesser-protected faces of initially grown gold nanostructure.     

A simple sol–gel technique for preparing hydroxyapatite nanopowders

HA powder was prepared using a sol–gel method with phosphoric pentoxide (P₂O₅) and calcium nitrate tetrahydrate (Ca(NO₃)₂·4H₂O). The effect of sintering temperatures on crystalline degree and composition of the HA phase, and also the effect of aging times on crystal size of the HA powder were studied using XRD and TEM. It was found that at sintering temperatures ranging from 600 to 900 °C, the dominant phase in the powders was HA with small amounts of calcium oxide and β-tricalcium phosphate (β-TCP) at 800 and 900 °C, and only HA phase was observed at 600 and 700 °C. 10–15 nm HA powders were obtained using this technique. This technique has an advantage over other sol–gel methods in more simple and shorter time because of no requiring pH value control and long hydrolysis time.     

Synthesis and characterisation of alumina fibres using organic/inorganic composite sol

Abstract

The polyvinyl butyral–Al(NO₃)₃ composite sols and alumina fibres were synthesised by the sol–gel process in an aqueous solution using the polyvinyl butyral (PVB) and Al(NO₃)₃.9H₂O (AN). The viscosity of PVB–AN composite sol increased with increasing AN content and aging time when it was laid at room temperature. The addition of AN leads to the formation of new weak peak and the deviation of diffraction angle to higher degrees according to the X-ray diffraction patterns (XRD). The exothermic peak of PVB disappeared and a weak endothermic peak was observed in differential scanning calorimetry curves of composite powders. The XRD pattern of fibres sintered at 1200°C showed the formation of α-alumina and the fibres showed smooth surface and uniform diameter.     

聚乙烯吡咯烷酮对羟基磷灰石结晶和形貌的影响

采用化学均相沉淀法,在水热条件下以Ca(NO3)2.4H2O和(NH4)2HPO4为原料,合成了具有特殊形貌的羟基磷灰石(HA)微球。在合成过程中加入聚乙烯吡咯烷酮(PVP)为模板剂,研究了PVP的加入和浓度对HA晶体形貌和粒径的影响。结果表明,PVP的加入改变了HA晶体的生长方式,颗粒是由针片状HA晶体组成的微球;HA颗粒的形貌和粒径可以通过调节PVP浓度来控制,当PVP浓度从0%(质量分数,下同)增加到12%时,HA颗粒的形貌逐渐由不规则的絮状团聚物转变为规整的微球,组成微球的结构单元也随PVP浓度的变化有所不同。     

Efficient and green oxidative degradation of methylene blue using Mn-doped ZnO nanoparticles (Zn1−xMnxO)

Mn-doped ZnO nanoparticles, Zn_1?xMn_xO, were synthesised by a polyethylene glycol (PEG) sol–gel method and the physicochemical properties of compounds were characterised by atomic absorption spectroscopy (AAS), energy-dispersive X-ray analysis, X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The catalytic degradation of an organic dye, methylene blue (MB), in the presence of Zn_1?xMn_xO as the catalyst and hydrogen peroxide (H₂O₂) as the oxidant at room temperature in water has been studied. Effects of oxidant, catalyst amount, catalyst composition, pH value of the solution and an OH-radical scavenging agent on the degree of the decomposition of MB dye were also studied.     

Surface modification of natural and synthetic hydroxyapatites powders by grafting polypyrrole

The modification of hydroxyapatite surface by grafting polypyrrole has been investigated with two hydroxyapatites (HA) powders. One is natural derived from bovine bone, it was prepared by calcination at 750 °C. The other is synthetic synthesized by the sol–gel method using Ca(NO₃)₂·4H₂O and P₂O₅. The presence of (C₄H₃N) _n polymeric fragment bound to HA surface was evidenced by infrared analysis. X-ray powder analysis has shown that the apatite structure remains unchanged during the surface modification. The thermogravimetric analysis has shown that the weight loss exhibited by HA increased from 8.7 to 47.8 and from 18.3 to 42.8 wt% for natural hydroxyapatite (NHA)/polypyrrole and synthetic hydroxyapatite (SHA)/polypyrrole, respectively, as the pyrrole solution concentration increased from 5 to 15 wt%. Grafting of polypyrrole on HA surface caused an increase in specific surface area up to 113 m²/g for SHA and up to 107 m²/g for NHA aged in 15 wt% pyrrole solution (HA/15Pyrrole). According to the results found for these two apatites, a mechanism of surface modification was proposed for the formation of N–H hydrogen bonds as the result of a reaction between the C₄H₅N organic reagent and OH^? ions of the HA.     

Structural,optical, electrical properties of new hybrid organic–inorganic NLO single crystal: bis(1H-benzotriazole) hexaaqua-zinc bis(sulfate) tetrahydrate (BZS)

A new hybrid organic–inorganic nonlinear (NLO) single crystal, Bis(1H-benzotriazole) hexaaqua-zinc bis(sulfate) tetrahydrate (BZS), has been successfully synthesized and the single crystals were grown by slow evaporation solution growth technique (SESG) using Millipore water as a solvent. The structure of the BZS crystal was solved and refined by single-crystal X-ray diffraction and demonstrates that the grown crystals belong to a triclinic system with the space group P-1. The asymmetric part of the titled compound contains isolated organic cation (C₆H₆N₃)₂, metallic cation [Zn(H₂O)₆]²⁺, sulfate anion (SO₄)^2? and free H₂O molecules. The interplay between the wide number of intermolecular interaction such as O–H···O, N–H···O, C–H···O and π–π stacking interactions were discussed. The optical transmittance spectrum shows that the crystal is excellent transmittance in the entire Vis–NIR region with the cutoff wavelength at 345 nm. The presences of expected functional groups were identified by Fourier transform infrared spectroscopy. The dielectric measurements were carried out at different temperature in the frequency range 100 Hz–5MHz. Furthermore, the studies of its third-order NLO properties using a Z-scan technique demonstrate that the BZS crystal possesses a strong reverse saturable absorption (RSA) and the self-focusing (SF) nature with large second order hyperpolarizability (γ?=?6.24?×?10^?34 esu). All the results indicate that BZS crystal might be the potential candidate for the third-order NLO applications.     

Controllable synthesis of gadolinium tungstate nanoparticles with different surfactants by precipitation route

In this paper, gadolinium tungstate Gd₂(WO₄)₃ nanoparticles were synthesized via a new approach based on the reaction between gadolinium nitrate hexahydrate and Na₂WO₄.2H₂O in water.   Besides, three surfactants such as ethylene diaminetetraacetic acid (EDTA), sodium dodecyl sulfate (SDS), and polyvinylpyrrolidone (PVP) were used to investigate their effects on the morphology and particle size of Gd₂(WO₄)₃ nanoparticles. According to the vibrating sample magnetometer, gadolinium tungstate Gd₂(WO₄)₃ nanoparticles indicated a paramagnetic behavior at room temperature. The as-synthesized nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), diffuse reflectance spectroscopy (UV–Vis), and energy dispersive X-ray microanalysis (EDX). To evaluate the catalytic properties of nanocrystalline gadolinium tungstate, the photocatalytic degradations of methyl orange under ultraviolet light irradiation were carried out.     

Preparation of hydroxyapatite ceramics by hydrothermal hot-pressing method at 300 °C

Hydroxyapatite (HA) ceramics were prepared by a hydrothermal hot-pressing (HHP) method at a low temperature (300 °C). DCPD (CaHPO₄·2H₂O) + Ca(OH)₂, OCP (Ca₈H₂(PO₄)₆·5H₂O) + Ca(OH)₂, DCPD + NH₃·H₂O, OCP + NH₃·H₂O or α-TCP (Ca₃(PO₄)₂) + NH₃·H₂O were used as the precursors. The mixture was treated by HHP under a condition of 300 °C/40 MPa. In sample DCPD + Ca(OH)₂ and OCP + Ca(OH)₂, the HA ceramics obtained showed a porous and homogenous microstructure, and the bending strength were 9.9 MPa and 10.9 MPa, respectively. In sample α-TCP+NH₃·H₂O, rod-like HA crystals produced. When the starting materials were DCPD + NH₃·H₂O, OCP + NH₃·H₂O, the HA particles produced exhibited plate-like features. It appeared that the plate-like HA particles stacked into a lamellar structure. The formation of the lamellar structure leads to a noticeable improvement in fracture property of the HA ceramic. The bending strength and the fracture toughness of the sample prepared from OCP and ammonia water reach 90 MPa and 2.3 MPam^1/2, respectively.     

Investigation of different factors towards synthesis of CuS spherical nanoparticles

Spherical CuS nanocrystals were synthesised via reflux (R) and hydrothermal (H) methods using copper acetate monohydrate (Cu (ac)₂·H₂O) and thioacetamide as precursors. This process was carried out in the absence and presence of cetyltrimethylammonium bromide (CTAB) and sodium dodecyl sulphate (SDS) surfactants. The products were characterised by using the methods of X-ray powder diffraction (XRD), scanning electron microscopy, energy-dispersive X-ray and transmission electron microscopy. According to XRD results, nanoparticles with the size of 16–23 nm were obtained. The effects of surfactant type, reaction time and reaction temperature on the morphology, yield, size and phase of the obtained products were investigated. According to this study, CTAB was more appropriate than SDS in obtaining uniform and spherical CuS nanoparticles.     

Coaxial electrospinning fabrication and electrochemical properties of LiFePO4/C/Ag composite hollow nanofibers

LiFePO₄/C/Ag composite hollow nanofibers were synthesized by calcination of the coaxial electrospun nanofibers with polyvinyl pyrrolidone (PVP) as core and [LiOH + Fe(NO₃)₃ + H₃PO₄]/PVP/AgNO₃ as shell. PVP was used as the electrospinning template and carbon source. During the calcination, LiFePO₄ precursor was transformed to LiFePO₄ while AgNO₃ and PVP were decomposed into silver and carbon. The morphology and properties of the as-prepared samples were characterized by X-ray diffraction, scanning electron microscopy, BET specific surface area analysis, electrochemical impedance spectroscopy and galvanostatic charge–discharge measurements. The results indicate that the mean diameter of as-prepared LiFePO₄/C/Ag composite hollow nanofibers is 154.5 ± 18.6 nm and the BET specific surface area is 119.14 m² g^?1. The addition of silver and carbon does not affect the structure of LiFePO₄, but improves its electrochemical performances. At the current density of 0.2 C, the initial discharge capacity of LiFePO₄/C/Ag hollow nanofibers electrode is 138.71 mAh g^?1, which is higher than that of LiFePO₄/C nanofibers electrode. The improved specific capacity may be attributed to increase electrode conductivity after the introduction of silver. The formation mechanism of the LiFePO₄/C/Ag composite hollow nanofibers was also proposed.     

Rapid synthesis of Ag@Ni core-shell nanoparticles using a microwave-polyol method

Mixtures of AgNO₃ and NiSO₄·6H₂O, NiCl₂·6H₂O, or Ni(NO₃)₂·6H₂O were reduced in ethylene glycol (EG) in the presence of NaOH and poly(vinylpyrrolidone) (PVP) under microwave (MW) heating for 10 min. Then, we succeeded in the synthesis of Ag core-Ni shell nanoparticles, denoted as Ag@Ni, in high yield. The formation of Ag@Ni particles was confirmed using energy dispersed X-ray spectroscopic (EDS) measurements and selected area electron diffraction (SAED) patterns. The growth mechanism of Ag@Ni is discussed. The UV-Vis spectra of Ag@Ni were similar to those of Ni particles.