Characterisation of HVOF sprayed Cr3C2-50(Ni20Cr) coating and the influence of binder properties on solid particle erosion behaviour

The coating Cr₃C₂ with 50 wt.% Ni20Cr deposited by high velocity oxy-fuel (HVOF) spray process was characterized in detail to investigate the effect of annealing on the solid particle erosion behaviour and understand the influence of the binder properties. Systematic characterization of the coating was carried out using electron microscopy (scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron probe microanalysis (EPMA)), X-ray diffraction (XRD), microindentation and nanoindentation techniques. The solid particle erosion tests were done on the as-sprayed coating and coatings annealed at 400 °C, 600 °C and 800 °C using silica erodent particles. The coefficient of restitution of the coated samples was also measured by WC ball impact tests to simulate dynamic impacts. The as-sprayed coating consisted of primary carbides and binder that was a mixture of amorphous and nanocrystalline phases. Annealing leads to recrystallisation of binder phase and precipitation of secondary carbides. The coating hardness and binder ductility change with annealing temperature. The erosion resistance improves with annealing up to 600 °C. In the as-sprayed coating, the amorphous phase, inter-splat boundaries and the elastic rebound characteristics affect the erosion response. While in the case of the coating annealed at 600 °C, the presence of ductile crystalline binder, fine carbide precipitates and embedment of erodent particles together improve solid particle erosion resistance.     

Annealing temperature effect on the corrosion parameters of autocatalytically produced Ni-P and Ni-P-Al2O3 coatings in artificial seawater

Ni-P and Ni-P-Al₂O₃ amorphous alloy coatings with 9.3 and 8.3 wt.% P respectively were obtained by autocatalytic deposition at 90 °C on carbon steel substrates. The effect of annealing temperature (100, 200, 300, 400 and 500 °C) upon the corrosion parameters of the coatings in artificial seawater with pH 5.0 and 8.1 at room temperature was evaluated by potentiodynamic polarisation and electrochemical impedance spectroscopy. It was found that deposits annealed at 400 and 500 °C presented an increase of the charge transfer resistance and negligible changes on samples annealed at lower temperature. Polarisation tests showed a charge transfer controlled anodic kinetics on both Ni-P and Ni-P-Al₂O₃ deposits and diffusion controlled cathodic reaction in artificial seawater at pH 5.0 and 8.1. The coatings did not present passive behaviour in the electrolytes and impedance measurements showed a single time constant for all cases with the lowest double layer capacitance (C_dl) for samples annealed at 400 and 500 °C. The best corrosion parameters were observed on Ni-P and Ni-P-Al₂O₃ coatings annealed at temperatures higher than 400 °C, which is the temperature where crystallisation of this kind of coatings takes place.     

Perpendicular magnetic anisotropy in 70 nm CoFe2O4 thin films fabricated on SiO2/Si(1 0 0) by the sol-gel method

Cobalt ferrite CoFe₂O₄ films were fabricated on SiO₂/Si(1 0 0) by the sol-gel method. Films crystallized at/above 600 °C are stoichiometric as expected. With increase of the annealing temperature from 600 °C to 750 °C, the columnar grain size of CoFe₂O₄ film increases from 13 nm to 50 nm, resulting in surface roughness increasing from 0.46 nm to 2.55 nm. Magnetic hysteresis loops in both in-plane and out-of-plane directions, at different annealing temperatures, indicate that the films annealed at 750 °C exhibit obvious perpendicular magnetic anisotropy. Simultaneously, with the annealing temperature increasing from 600 °C to 750 °C, the out of plane coercivity increases from 1 kOe to 2.4 kOe and the corresponding saturation magnetization increases from 200 emu/cm³ to 283 emu/cm³. In addition, all crystallized films exhibit cluster-like structured magnetic domains.     

Structural, optical and electrical properties of CuIn5S8 thin films grown by thermal evaporation method

Stoichiometric compound of copper indium sulfur (CuIn₅S₈) was synthesized by direct reaction of high purity elemental copper, indium and sulfur in an evacuated quartz tube. The phase structure of the synthesized material revealed the cubic spinel structure. The lattice parameter (a) of single crystals was calculated to be 10.667 Å. Thin films of CuIn₅S₈ were deposited onto glass substrates under the pressure of 10⁻⁶ Torr using thermal evaporation technique. CuIn₅S₈ thin films were then thermally annealed in air from 100 to 300 °C for 2 h. The effects of thermal annealing on their physico-chemical properties were investigated using X-ray diffraction (XRD), Energy-dispersive X-ray spectroscopy (EDX), scanning electron microscope (SEM), optical transmission and hot probe method. XRD studies of CuIn₅S₈ thin films showed that as-deposited films were amorphous in nature and transformed into polycrystalline spinel structure with strong preferred orientation along the (3 1 1) plane after the annealing at 200 °C. The composition is greatly affected by thermal treatment. From the optical transmission and reflection, an important absorption coefficient exceeds 10⁴ cm⁻¹ was found. As increasing the annealing temperature, the optical energy band gap decreases from 1.83 eV for the as-deposited films to 1.43 eV for the annealed films at 300 °C. It was found that CuIn₅S₈ thin film is an n-type semiconductor at 300 °C.     

Effect of annealing temperature on the structure and optical properties of sputtered TiO2 films

TiO₂ thin films were deposited by DC reactive magnetron sputtering. Some TiO₂ thin films samples were annealed for 5 min at different temperatures from 300 to 900 °C. The structure and optical properties of the films were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (SEM) and ultraviolet-visible (UV-vis) spectrophotometry, respectively. The influence of the annealing temperature on the structure and optical properties of the films was investigated. The results show that the as-deposited TiO₂ thin films are mixtures of anatase and rutile phases, and possess the column-like crystallite texture. With the annealing temperature increasing, the refractive index and extinction coefficient increase. When the annealing temperature is lower than 900 °C, the anatase phase is the dominant crystalline phase; the weight fraction of the rutile phase does not increase significantly during annealing process. As the annealing temperature rises to 900 °C, the rutile phase with the large extinction coefficient becomes the dominant crystalline phase, and the columnar structure disappears. The films annealed at 300 °C have the best optical properties for the antireflection coatings, whose refractive index and extinction coefficient are 2.42 and 8 × 10⁻⁴ (at 550 nm), respectively.     

Effect of buffer growth temperature on crystalline quality and optical property of In0.82Ga0.18As/InP grown by LP-MOCVD

In_0.82Ga_0.18As epilayers were grown by LP-MOCVD on InP (1 0 0) substrates with two-step growth method. It was analyzed that growth temperature of buffer layer exerted an influence on its crystalline quality and optical property, which were characterized by X-ray diffraction, scanning electron microscopy, and photoluminescence. The experiments showed that the crystalline quality and the optical property of the In_0.82Ga_0.18As epilayers had close relation to the growth temperature of buffer layer and the optimum buffer's growth temperature was about 450 °C.     

Effect of air annealing on mechanical properties and structure of amorphous B4C films

Amorphous B₄C films were prepared by magnetron sputtering of the hot-pressed B₄C target in different regimes. Hardness, intrinsic stress and film structure were investigated in dependence on the annealing temperature in air.Changes in the film structure and composition were investigated by Raman spectroscopy, confocal microscopy, and electron probe microanalysis. It has been shown that an annealing at 500 °C for 1 h leads to stress reduction, slight thickness decrease and increase of film hardness. However already at 600 °C the film oxidation proceeds very intensively with formation of the phases of boron oxide and amorphous carbon in the surface layer. The thickness of the film decreases quickly.The film oxidation is accompanied by formation of numerous carbon hillocks and redistribution of film material after annealing in furnace at 500 and especially 600 °C. The oxidation of a-B₄C films as well as of the crystalline bulk samples starts in some locations and has clearly pronounced heterogeneous character that indicates heterogeneous structure of amorphous films as well as of bulk crystalline samples.Annealing in air for a long period shifts down the onset of formation of hillocks to 400 °C and changes in film morphology to 300 °C. Thus the upper temperature limit for application of a-B₄C films in air depends also on the exposure time at the operation temperature.     

P-type transparent conducting SnO2:Zn film derived from thermal diffusion of Zn/SnO2/Zn multilayer thin films

Highly transparent, p-type conducting SnO₂:Zn thin films are prepared from the thermal diffusion of a sandwich structure of Zn/SnO₂/Zn multilayer thin films deposited on quartz glass substrate by direct current (DC) and radio frequency (RF) magnetron sputtering using Zn and SnO₂ targets. The deposited films were annealed at various temperatures for thermal diffusion. The effect of annealing temperature and time on the structural, electrical and optical performances of SnO₂:Zn films was studied. XRD results show that all p-type conducting films possessed polycrystalline SnO₂ with tetragonal rutile structure. Hall effect results indicate that the treatment at 400 °C for 6 h was the optimum annealing parameters for p-type SnO₂:Zn films which have relatively high hole concentration and low resistivity of 2.389 × 10¹⁷ cm^− 3 and 7.436 Ω cm, respectively. The average transmission of the p-type SnO₂:Zn films was above 80% in the visible light range.     

Phase transformations in face centered cubic (Al0.32Cr0.68)2O3 thin films

Face centered cubic (Al_0.32Cr_0.68)₂O₃ thin films have been annealed in the temperature range of 500–1000 °C during 2–8 h. The fcc structure of the film remains intact when annealed at temperatures up to 700 °C for 8 h. X-ray diffraction and transmission electron microscopy show the onset of phase transformation to corundum phase alloys in the sample annealed at 900 °C for 2 h, where annealing at 1000 °C for 2 h results in complete phase transformation to α-(Al_0.32Cr_0.68)₂O₃. In-plane and out-of-plane line scans performed in EDX TEM and θ/2θ XRD patterns did not show any phase separation into α-Cr₂O₃ and Al₂O₃ prior and after the annealing. The apparent activation energy of this process is 380–480 kJ/mol as determined by the Johnson–Mehl–Avrami model.     

Atmospheric pressure chemical vapour deposition and characterisation of crystalline InTaO4, InNbO4 and InVO4 coatings

The possibilities to grow crystalline complex InTaO₄, InNbO₄ and InVO₄ coatings as well as single oxide layers In₂O₃, Ta₂O₅, Nb₂O₅, and VO_x were investigated using aerosol assisted atmospheric pressure chemical vapour deposition technique. Indium(III) and niobium(IV) tetramethylheptanedionates, tantalum(V) tetraethoxyacethylacetonate and vanadium(III) acethylacetonate were used as precursors, monoglyme and toluene as solvents. The influence of deposition conditions and solution composition on elemental and phase compositions of layers was studied. Indium tantalate layers containing pure monoclinic InTaO₄ phase were obtained ex-situ, i.e., after high-temperature (800 °C) annealing of layers grown at lower temperature (500 °C). Films containing pure orthorhombic indium vanadate or monoclinic indium niobate phase may be prepared using both in-situ (600 °C) or ex-situ (deposition at 400 °C, annealing at 800 °C) approaches. Under optimised deposition conditions and solution compositions, Ni-doped InVO₄ and InTaO₄ films were also deposited and their photocatalytic activity was tested.     

Investigation on thermal and microstructural characterization of the TeO2-WO3 system

Thermal and microstructural characterization of the TeO₂-WO₃ binary system was accomplished by applying differential thermal analysis (DTA), X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. Different compositions of the (1 − x)TeO₂-xWO₃ system, where x varies between 0.02 and 0.80 in molar ratio were studied. The samples were prepared by melting high purity powder mixtures of TeO₂ and WO₃ in a platinum crucible with a closed lid at 750 °C for 30 min and quenching in water bath. The glass forming range of the binary system was detected as 0.04 ≤ x ≤ 0.35 in molar ratio. As-cast samples were heat-treated above the crystallization peak temperatures at 550 °C for 24 h to obtain thermal stability and the phase stability of the binary system was investigated by performing systematical thermal, phase and microstructural characterizations with the heat-treated samples. The eutectic reaction of the binary system was detected at 617 ± 3 °C, the endothermic reaction indicating the phase transformation reaction of WO₃ from orthorhombic to tetragonal was determined at 743 ± 1 °C. α-TeO₂ and orthorhombic WO₃ crystalline phases were found to be present in the final structure when the total crystallization was achieved. Microstructural characterization of the TeO₂-WO₃ system was realized for a wide compositional range for the first time in the literature.     

Preparation of CuIn1−xGaxS2 (x = 0.5) flowers consisting of nanoflakes via a solvothermal method

CuIn_1−xGa_xS₂ (x = 0.5) flowers consisting of nanoflakes were successfully prepared by a biomolecule-assisted solvothermal route at 220 °C for 10 h, employing copper chloride, gallium chloride, indium chloride and l-cysteine as precursors. The biomolecule l-cysteine acting as sulfur source was found to play a very important role in the formation of the final product. The diameter of the CuIn_0.5Ga_0.5S₂ flowers was 1-2 μm, and the thickness of the flakes was about 15 nm. The obtained products were characterized by X-ray diffraction (XRD), energy dispersion spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction spectroscopy (SAED), and UV-vis absorption spectroscopy. The influences of the reaction temperature, reaction time, sulfur source and the molar ratio of Cu-to-l-cysteine (reactants) on the formation of the target compound were investigated. The formation mechanism of the CuIn_0.5Ga_0.5S₂ flowers consisting of flakes was discussed.     

N-doped Sb2Te phase change materials for higher data retention

Crystallization temperatures of the Sb₂Te films increase remarkably from 139.4 °C to 223.0 °C as the N₂ flow rates increasing from 0 sccm to 1.5 sccm. Electrical conduction activation energies for amorphous and crystalline states increase by doping nitrogen. A small amount of nitrogen atoms can locate at interstitial sites in the hexagonal structure, generating a strain field, and improving the thermal stability of amorphous state. The best 10-years lifetime at temperature up to 141 °C is found in Sb₂TeN₁ films. Doping excessively high nitrogen in Sb₂Te film will form nitride and make Te separate out. As a result, the activation energy for crystallization decreases instead, accompanying with the deterioration of thermal stability. The power consumption of PCRAM test cell based on Sb₂TeN₁ film is ten times lower than that of PCRAM device using Ge₂Sb₂Te₅ films.     

A new temperature stable microwave dielectric ceramics: ZnTiNb2O8 sintered at low temperatures

The phases, microstructure and microwave dielectric properties of ZnTiNb₂O₈-xTiO₂ composite ceramics with different weight percentages of BaCu(B₂O₅) additive prepared by solid-state reaction method have been investigated using the X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy-dispersive spectroscopy (EDS). The results showed that the microwave dielectric properties were strongly dependent on densification, grain sizes and crystalline phases. The sintering temperature of ZnTiNb₂O₈ ceramics was reduced from 1250 °C to 950 °C by doping BaCu(B₂O₅) additive and the temperature coefficient of resonant frequency (τ_f) was adjusted from negative value of −52 ppm/°C to 0 ppm/°C by incorporating TiO₂. Addition of 2 wt% BaCu(B₂O₅) in ZnTiNb₂O₈-xTiO₂ (x = 0.8) ceramics sintered at 950 °C showed excellent dielectric properties of ?_r = 38.89, Q × f = 14,500 GHz (f = 4.715 GHz) and τ_f = 0 ppm/°C, which represented very promising candidates as LTCC dielectrics for LTCC applications.     

Investigation of structure and magnetization reversal in mechanically alloyed SmCo6.8Zr0.2 magnets

Nanocrystalline SmCo_6.8Zr_0.2 permanent magnets are prepared by intensive milling and subsequent annealing. XRD patterns of the samples annealed at 600 °C and 700 °C show a single SmCo₇ phase with TbCu₇ structure, while the SmCo₇ phase decomposes into a mixture of Sm₂Co₁₇ and Co₂₃Zr₆ phase at higher annealing temperatures. The highest coercivity and energy product of about 2.06 T and 9.5MGOe are obtained in the sample annealed at 700 °C for 10 min. Further analysis reveals that a very strong inter-grain exchange coupling is observed in samples annealed at 700 °C for 3 (SZ-3) and 10 (SZ-10) min, indicating by the high remanence ratio and positive δm in henkel-plot. It was supposed that the magnetization reversal process is controlled by domain wall pinning.     

Structure and mechanical properties of TiAlSiN/Si3N4 multilayer coatings

TiAlSiN/Si₃N₄ multilayer coatings which have different separate layer thicknesses of TiAlSiN or Si₃N₄ were deposited onto glass sheets, single-crystal silicon wafers and polished WC-Co substrates by reactive magnetron co-sputtering. The morphology, crystalline structure and thickness of the as-prepared multilayer coatings were characterized by TEM, SEM, XRD and film thickness measuring instrument. The mechanical properties of the coatings were evaluated by a nanoindenter. The effects of monolayer thickness on the microstructure and properties of TiAlSiN/Si₃N₄ multilayer coatings were explored. The coatings showed the highest hardness when the thickness of Si₃N₄ and TiAlSiN monolayers was 0.33 nm and 5.8 nm, respectively. The oxidation characteristics of the coatings were studied at temperatures ranging from 700 °C to 900 °C for oxidation time up to 20 h in air. It was found that the coatings displayed good oxidation resistance.     

Enhanced photoluminescence of GdPO4:Tb under VUV excitation by controlling ZnO content and annealing temperature

High-quality Zn-free and added GdPO₄:Tb³ green phosphors, i.e., fine size as well as smooth and spherical morphologies, were synthesized by ultrasonic spray pyrolysis. The influence of Zn²⁺ content and annealing temperature on the photoluminescence properties of the GdPO₄:Tb³ phosphors annealed at 800-1100 °C was investigated. The addition of Zn²⁺ for Gd³⁺ was highly effective for improving the photoluminescence properties of GdPO₄:Tb³. The Zn added GdPO₄:Tb³ phosphors with Zn/Gd = 0.045/0.805 showed the strongest emission of the prepared phosphors. The emission intensity at 544 nm for the GdPO₄:Tb³ phosphors with Zn/Gd = 0.045/0.805 annealed at 900 °C was 496% stronger than that at 800 °C.     

Oxidation behavior of Ti3AlC2 at 1000-1400 °C in air

The isothermal oxidation behavior of bulk Ti₃AlC₂ has been investigated at 1000-1400 °C in air for exposure times up to 20 h by means of TGA, XRD, SEM and EDS. It has been demonstrated that Ti₃AlC₂ has excellent oxidation resistance. The oxidation of Ti₃AlC₂ generally followed a parabolic rate law with parabolic rate constants, k_p that increased from 4.1×10⁻¹¹ to 1.7×10⁻⁸ kg² m⁻⁴ s⁻¹ as the temperature increased from 1000 to 1400 °C. The scales formed at temperatures below 1300 °C were dense, adherent, resistant to cyclic oxidation and layered. The inner layer of these scales formed at temperatures below 1300 °C was continuous α-Al₂O₃. The outer layer changed from rutile TiO₂ at temperatures below 1200 °C to a mixture of Al₂TiO₅ and TiO₂ at 1300 °C. In the samples oxidized at 1400 °C, the scale consisted of a mixture of Al₂TiO₅ and, predominantly, α-Al₂O₃, while the adhesion of the scales to the substrates was less than that at the lower temperatures. Effect of carbon monoxide at scale/substrate was involved in the formation of the continuous Al₂O₃ layers.     

Thermal stability of bulk Zr2Al4C5 ceramic at elevated temperatures

Thermal expansion analysis is applied to the study of phase segregation of Zr₂Al₄C₅ at elevated temperatures (20-2000 °C) under flowing argon. Such information would be useful for the detection of phase decomposition temperature and thermal stability of materials. The detected phase-decomposition temperature of Zr₂Al₄C₅ is approximately 1900 °C. The presented thermal expansion analysis results are in good agreement with the X-ray diffraction (XRD) and SEM results. The results indicate that Zr₂Al₄C₅ is susceptible to decomposition through sublimation of high vapor pressure of Al and weaker covalent bonds between ZrC slabs and Al₄C₃ layers. Thus, minimal amounts of Al, Zr₂Al₃C₅, Al₄C₃ and ZrC form on the surface layer. Zr₂Al₃C₅ further decomposes to ZrC_1 − x and Al₄C₃ at 2000 °C. However, the amount of decomposing phase slowly increases, and the structural shape of bulk Zr₂Al₄C₅ ceramic is always kept stable during heat treatment.     

Synthesis, structure and optical properties of CoAl2O4 spinel nanocrystals

CoAl₂O₄ nanocrystals were synthesized by sol-gel method using citric acid as a chelating agent at low temperature. The as-synthesized samples were characterized by thermal analysis, X-ray powder diffraction, infrared spectroscopy and transmission electron microscopy. The results show that CoAl₂O₄ spinel is the only crystalline phase with a size of 10-30 nm in the temperature range 500-1000 °C. The temperature dependence of the distribution of Al³⁺ and Co²⁺ ions in the octahedral and tetrahedral sites in nanocrystals was investigated by X-ray photoelectron spectroscopy (XPS). It is observed that the inversion parameter decreases with increasing annealing temperature. Analysis of the absorption properties indicates that Co²⁺ ions are located in the tetrahedral sites as well as in the octahedral sites in the CoAl₂O₄ nanocrystals. The origin of the green color (300-500 nm absorption band) should be due to the octahedrally coordinated Co²⁺ ions.