Structural investigation of nanohydroxyapatite doped with Y3+ and F– ions

Abstract

Pure and 2·5 mol.-%Y³⁺ and F^– doped nanohydroxyapatites were synthesised by a precipitation method and sintered at 900 and 1100°C to investigate their densification and structure. X-ray diffraction and Fourier transform infrared spectroscopy methods were performed to identify the presence of phases and bonds after the sintering respectively. Densification of hydroxyapatite was improved by the addition of these ions. No second phases were observed by X-ray diffraction method. Structure of the materials was hexagonal. Fourier transform infrared spectroscopy investigations showed that the Y³⁺ and F^– doped hydroxyapatites had F^– bonds in addition to OH^– bonds after the sintering.     

Investigation of tensile strength of hydroxyapatite with various porosities by diametral strength test

Abstract

It is appropriate to administer the diametral test to biomedical materials used in dental applications because stresses formed on dental implants are similar to those that formed in this test. To show this similarity, an experimental study of diametral strength testing of hydroxyapatite was performed. The influence of porosity on hydroxyapatite was investigated experimentally to determine how the diametral strength was affected. Hydroxyapatite was air sintered at 1100°C for 1 h with porosities ranging from 1 to 32%. The results indicated that hydroxyapatite with improved densification had higher diametral strength values. X-ray diffraction analysis showed that sintered samples were pure hydroxyapatite.     

Effects of Mg doping on sol–gel derived nanocrystalline hydroxyapatite thin films

Abstract

Both pure and Mg doped thin films were fabricated by sol–gel dip coating. The films were sintered either at 800 or 1000°C. The average grain size of the films was significantly affected by Mg substitution in the hydroxyapatite (HA) structure and change in the sintering temperature. The grains were considerably larger in the films sintered at higher temperatures. In addition, Mg doped films contained significantly larger grains compared to undoped HA films. Mg doping also caused rodlike grains at 800°C, and led to whitlockite (β-TCP) formation at 1000°C. The ratio of the existing phases was estimated as β-TCP/HA=27 : 73. All the films had rough surfaces with high porosity. It was also observed that undoped films had higher surface roughness than Mg doped ones.     

Quasicrystalline phase formation during heat treatment in mechanically alloyed Al65Cu20Fe15 alloy

Abstract

Quasicrystalline phase formation during heat treatment in the mechanically alloyed Al₆₅Cu₂₀Fe₁₅ powders was studied by X-ray diffraction (XRD) and differential scanning calorimeter (DSC). The mechanical alloying was performed at speed of 300 rev min^–1 for times up to 70 h. It was found that mechanical alloying of the Al₆₅Cu₂₀Fe₁₅ powders did not result in the quasicrystalline (QC) icosahedral phase (i-phase) formation. The long time milling resulted in the formation of a cubic Al (Cu,Fe) solid solution phase (β-phase). The cubic Al (Cu,Fe) solid solution identified as β-phase was observed to be present as one of the major phases in the Al₆₅Cu₂₀Fe₁₅ alloy. The formation of the quasicrystalline icosahedral phase (i-phase) was only observed for short time milled powders after additional annealing at temperature above 500°C. The present investigation also showed that a tetragonal Al₂Cu phase (θ-phase) forms with short time milling. The tetragonal Al₇Cu₂Fe₁ phase (w-phase) was observed after heat treatment of the short time milled and unmilled powders. The present investigation indicated that an effective process to prepare the quasicrystalline materials was using a combination of short time milling and subsequent annealing.     

Oxide ionic conductivity and crystallographic properties of tetragonal type Bi2O3-based solid electrolyte doped with Ho2O3

Abstract

In the present work, the authors have investigated the binary system of (Bi₂O₃)_1–x(Ho₂O₃)_x. For the stabilisation of the tetragonal type solid solution, small amounts of Ho₂O₃ were doped into the monoclinic Bi₂O₃ via solid state reactions in the stoichiometric range 0·01≤x≤0·1. The crystal formula of the formed solid solution was determined as Bi(III)_4–4xHo(II)_4xO_6–2xVo_(2+2x) (where Vo is the oxide ion vacancy) according to the XRD and SEM microprobe results. In the crystal formula, stoichiometric values of x were 0·04≤x≤0·08, 0·03≤x≤0·09, 0·02≤x≤0·09 and 0·04≤x≤0·09 for annealing temperatures at 750, 800, 805 (quench) and 760°C (quench) respectively. The four probe electrical conductivity measurements showed that the studied system had an oxide ionic type electrical conductivity behaviour, which is increased with increasing dopant concentration and temperature. The obtained solid electrolyte system has an oxygen non-stoichiometry characteristic, and it contains O^2– vacancies, which have disordered arrangements in its tetragonal crystal structure. The increase in the amount of Ho₂O₃ doping and temperature causes an increasing degree of the disordering of oxygen vacancies and a decrease in the activation energy E_a.     

Synthesis and photochemical properties of Cu2+ doped layered hydrogen titanate

Cu²⁺ doped layered hydrogen titanate was prepared by the calcination of K₂CO₃, TiO₂ and CuO mixtures with the K₂CO₃:TiO₂:CuO molar ratio of 1:2.5(1−x):2.5x at 1200°C for 5 h followed by an ion-exchange reaction in 1 M HCl solution. The crystalline phase changed from monoclinic hydrogen tetratitanate to an orthorhombic lepidocrocite-type hydrogen titanate by increasing the amount of Cu²⁺ doped. Both compounds could be excited by visible light irradiation (λ>400 nm) and were capable of hydrogen gas evolution from an aqueous methanol solution, where the photocatalytic activity of Cu²⁺ doped hydrogen tetratitanate was slightly greater than that of Cu²⁺ doped lepidocrocite-type hydrogen titanate. The photocatalytic activity of Cu²⁺ doped hydrogen tetratitanate was enhanced by constructing Pt and TiO₂ pillars in the interlayer, and the incorporation of Pt in Cu²⁺ doped hydrogen tetratitanate enabled the cleavage of water into hydrogen and oxygen by irradiating visible light (λ>400 nm) without a sacrificial hole acceptor.     

Growth of Cu2+ and Mg2+ doped nonlinear optical LATF crystals and their characterization

Single crystals of pure, Cu²⁺ and Mg²⁺ doped l-arginine trifluoroacetate (LATF) have been grown by the temperature lowering method. The presence of Cu²⁺ and Mg²⁺ was determined by atomic absorption spectroscopy (AAS). Single crystal X-ray diffraction studies were performed to calculate the lattice parameters of the pure and doped crystals. Absorption of these crystals was analyzed and the result confirms that they possess low absorption in the range 230–1100 nm. Thermal analysis (TGA, DTA) and Fourier transform infrared (FTIR) spectroscopy were carried out to investigate the thermal behavior and molecular vibrations of these crystals, respectively. The second harmonic generation (SHG) measurement reveals the NLO properties of pure and doped crystal. Surface morphologies of these crystals were also observed and studied in detail by atomic force microscopy.     

TiO2载Cu2+、Zn2+无机抗菌剂的制备及性能研究

采用固相合成法制备以TiO2为载体,以Cu2 、Zn2 为主要抗菌成分的无机抗菌剂,研究了制备条件及Cu2 、Zn2 含量对抗菌性能的影响,结果表明:当热处理温度为450～600℃,保温时间为2h,Cu2 和Zn2 质量百分含量比为(0.66～1.18):(2～3)时,样品均具有较好的抗菌效果;具有最好抗菌效果的样品中,TiO2以锐钛矿相存在,同时羟基氧的生成及Cu2 和Cu 的共存,使得样品具有良好的抗菌效果.     

Quantification of precipitate fraction in maraging steels by X-ray diffraction analysis

Abstract

Quantification of precipitate fraction, a critical step in modelling precipitation hardening, is difficult to carry out for maraging steels because of the small precipitate size and its low volume fraction. A method is proposed in the present work to estimate the precipitate fraction in an 18 wt-%Ni C250 maraging grade based on simple X-ray diffraction (XRD) analysis. The estimation gives reasonable values of precipitate fraction, which increases when aging proceeds. The precipitate formed at 427°C may be of a type that has not been reported before. The method proposed may be applicable to other precipitate hardened alloys. The amount of reverted austenite formed was also estimated when applicable.     

Analysis of reaction layer formed on steel strips during hot dip aluminising

Abstract

Aluminised steel sheets are currently used in many applications where the surface properties of aluminium combined with the formability, mechanical strength, and economic advantages of sheet material are obtained. During aluminising by hot dipping, an intermetallic reaction occurs due to diffusion between the aluminium bath and the steel sheet. The phases formed within the intermetallic layer and its thickness are important for determining the behaviour of the coating. In the present work, low alloy, medium carbon, low carbon 9Γ2C (9G2S), and low carbon steel sheets are used for hot dipping in a commercial purity aluminium bath. The temperatures used for hot dipping were 710 and 770°C and the immersion times were 2, 4, and 6 min. The results indicate that the thickness of the intermetallic layer X increases with increasing bath temperature and immersion time t. The variation of X with t followed the relationship X=Ktⁿ, where the constant K and the exponent n were found to depend on the carbon content and on the total alloying element content in the steel strip. With increasing total alloying elements, the thickness decreased. Analysis of the reaction layer indicates the formation of FeAl₂ in most cases in addition to FeAl₃, Fe₂Al₅, and Fe₂Al₃.     

Formation of zinc oxide nanoparticles by mechanochemical reaction

Abstract

The synthesis of zinc oxide (ZnO) nanocrystallites by mechanochemical reaction of ZnCl₂ and Na₂CO₃ with NaCl as diluent and following thermal treatment was investigated using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Calcination of the as milled powder at 600°C in air and removal of NaCl through washing formed ZnO nanocrystallites with an average crystal size of ~ 21 nm, which increased with increasing thermal treatment temperature. Milling time and NaCl/ZnCl₂ molar ratio exerted prominent effects on the crystal size of the ZnO nanoparticles. The mechanism of nanocrystallite growth is discussed.     

Electronic absorption spectrum of Cu2+ ions doped in lithium caesium sulphate single crystal

Copper-doped lithium caesium sulphate single crystals were grown by the slow evaporation method at room temperature. The electronic absorption spectra were recorded both at room and liquid-nitrogen temperatures on a Cary-2300 spectrophotometer. A crystal of thickness about 1 mm was found suitable in the present work. Three bands were observed at room temperature, two in the near-infrared region at 7813 cm⁻¹ and 9901 cm⁻¹ and one in the visible region at 12987 cm⁻¹. When the crystal was cooled to liquid-nitrogen temperature, changes in intensity and band position were observed. From the magnitude and relative position of the bands a successful interpretation of all the observed bands has been made and identified as those belonging to Cu²⁺ ion in tetragonal symmetry. The crystal field and tetragonal field parameters are derived. The observed and calculated energies are in good agreement.     

Quantitative X-ray diffraction analysis of development of Z phase in 12%Cr–Nb–V–N steel

Abstract

To study the evolution of nitrides (Nb,V)N, (V,Nb)N and Cr₂N, and in particular the formation of the Z phase Cr(V, Nb)N, a model alloy with composition similar to that of 12%Cr steels for high temperature applications, microalloyed with Nb and V but with a very low carbon content, has been designed. A quantitative determination of the volume fractions of the extracted nitrides that had formed after aging treatments at 650°C for up to 10 000 h was carried out by an X-ray diffraction procedure, based on the Rietveld approach. The investigation of the Z phase evolution by the Johnson–Mehl–Avrami–Kolmogorov kinetics at 650 and 700°C revealed that, as the kinetic exponent is very close to unity, the formation mechanism of this phase is not associated with a conventional process of nucleation but hints at a gradual diffusion controlled transformation of the pre-existing V and Nb nitrides.     

Microstructural and electrical characteristics of SiO2 doped ZnO-Bi2O3 varistors

Varistors in the new system ZnO-Bi₂O₃-SiO₂ were prepared through conventional ceramic processing route. The effect of sintering temperature and time (0·5 h to 2 h between 1000° and 1250°C) on the microstructure and current/voltage characteristics of the varistors of the new system were investigated and the results were compared with those of ZnO-Bi₂O₃ system varistors prepared. An increase in nonlinear coefficient (α) value was observed in the SiO₂ added varistors. The microstructure and the phase of the varistors were examined by means of SEM and XRD. The Zn₂SiO₄ spinel phase was found to be present in the intergranular region. The grain growth exponent was determined to be 2·5±0·2 and the activation energy for the ZnO grain growth was estimated to be 251±11 kJ/mol. These values were compared with those estimated for ZnO-Bi₂O₃ system varistors.     

Multicolor luminescence from transition metal ion (Mn2+ and Cu2+) doped ZnS nanoparticles

Mn and Cu doped ZnS nanoparticles in powder form were prepared by a simple solvothermal route. Particle size and crystal structure of the products were investigated through X-ray diffraction study revealing the formation of cubic ZnS nanoparticles of average diameter 2.5 nm. Particle size was also verified by the high resolution transmission electron microscopic images. Blue emission at approximately 445 nm was observed from the undoped sample, which was attributed to the presence of large surface defects. With increasing doping concentration the defect related emission gradually quenches and subsequently the impurity related emissions appeared. Mn doped samples exhibited orange emission at approximately 580 nm which may be attributed to the transition between (4)T1 and (6)A1 energy levels of the Mn2+ 3d states. Whereas, the Cu doped ZnS nanoparticles exhibited a red shifted strong blue emission at approximately 466 nm which is attributed to the transition of the electrons from the surface states to the 't2' levels of Cu impurities.     

Effects of processing parameters on direct laser sintering of multicomponent Cu based metal powder

Abstract

Direct laser sintering of a multicomponent Cu based metal powder was successfully processed through the mechanism of liquid phase sintering with partial melting of the powder. The effects of processing parameters such as laser power, scan speed, scan line spacing and layer thickness on the densification and microstructural evolution of the laser sintered powder were investigated. It was found that with increasing laser power or decreasing scan speed, the density of the sintered parts increased and the microstructures became denser. However, the combination of higher laser powers (>400 W) and higher scan speeds (≥0·06 ms^?1) gave rise to 'balling' effect. A successive transition from discontinuous scan tracks to coherently joined ones occurs with decreasing scan line spacing. Lowering the thickness of the powder layer promises an improvement in bonding coherence between sintered layers. A single factor termed 'energy density by volume' is defined to evaluate the combined effect of various processing parameters on the density of laser sintered powder. With increasing the energy density by volume up to ～0·16 kJ mm^?3, the densification rate is relatively high. However, with intensifying the energy density over ～0·23 kJ mm^?3, the mechanism of particle bonding may change into full melting/solidification, leading to a decrease in the sintered density.