Structural and phase transformation behaviour of electroless Ni-W-Cr-P alloy coatings on stainless steel

Ni-W-Cr-P alloy coatings were prepared by electroless deposition on stainless steel. The effects of heat-treatment on the structure and phase transformation behavior, microhardness of the Ni-W-Cr-P alloy coatings were mainly investigated. XRD analysis shows that as-deposited Ni-W-Cr-P coatings were microcrystalline; the precipitation of Ni₃P was observed at the annealing temperature of 400°C; after heat-treatment at 500°C the crystallization of Ni₃P and Ni was near completion; at 600°C new phase Cr_1.12Ni_2.88 was observed and Ni₃P began to decompose. Cr_1.07Fe_18.93 and Ni₁₇W₃ were formed when heated at 700°C, and Ni₃P was not found. With increasing temperature to 800°C, FeNi₂P and Cr₄Ni₁₅W were the only two dominant phases. The experimental results reveal that with an increase in the annealing temperature, micro-hardness of the Ni-W-Cr-P alloy coatings increased, reached the maximum value at 700°C, and then decreased slightly. Annealing temperature dependence of the microhardness and corrosion resistance of the coatings was also observed. The related strengthening mechanism in the electroless deposited Ni-W-Cr-P alloy coatings is also discussed.     

Microstructural characterization of a carbonitrided heat resisting alloy using focused ion beam-based techniques

Abstract

An austenitic Fe–25Cr–20Ni (wt.%) alloy was first nitrided in N₂–H₂ then carburised at 1000°C. The nitridation produced lamellar internal precipitates of Cr₂N which grew by discontinuous precipitation at a recrystallised austenite boundary formed at the precipitation front. Subsequent carburisation converted the Cr₂N to a mixture of chromium-rich M₇C₃+CrN, and released nitrogen into the austenite matrix. The submicron CrN precipitates were stabilized by a matrix supersaturated with nitrogen and exhibited a strong orientation relationship with the surrounding austenite. The rejected nitrogen diffused deeper into the alloy to form new, more finely spaced Cr₂N lamellae. Carbon diffusion overtook the nitride structure and precipitated finely spaced, lamellar M₂₃C₆ by a discontinuous precipitation process. This process is available to the carbides only when a prior boundary is present. This phenomenon, and the ability of nitridation to form a boundary and the inability of carburisation to do so, are interpreted using the energetics of nucleation.     

A study on the influence of Mo, Al and Si additions on the microstructure of annealed dual phase Cr–Ta alloys

The effects of additions of 5 at.% Mo, Al and Si on the long-term annealed microstructures of a two phase Cr–Cr₂Ta alloy have been studied. Following 200 h at 1300 °C, the lamellar eutectic constituent of all the alloys disintegrated into discrete particles of the Laves phase embedded within a Cr-rich solid solution phase, along with the formation of fine Laves phase precipitates. One of the predominant differences between the three alloying additions was the extent of the C14 to C15 polytypic transformation of the Cr₂Ta-based Laves phase. With Mo and Al additions, the Cr₂Ta Laves phase transformed from C14 to either C15 or intermediate hexagonal polytypes following 200 h annealing at 1300 °C. In contrast, Si additions stabilised the C14 polytype, with no transformation to other polytypes observed after prolonged annealing at 1000, 1100 and 1300 °C.     

Surface and catalytic properties of CuO/MgO system doped with K2O and Cr2O3

The effects of doping of CuO/MgO system with K₂O or Cr₂O₃ (1–6 wt.%) on its surface and catalytic properties were investigated. The analytical techniques employed were XRD, nitrogen adsorption at −196 °C and decomposition of H₂O₂ at 30–50 °C. The results revealed that K₂O-treatment of the system investigated, followed by calcinations at 400 °C resulted in the conversion of some of the surface copper oxide into potassium coprate K₃Cu₅O₄ phase whose diffraction lines disappeared upon heating at 500 °C. Chromium oxide-doping did not lead to the formation of any copper oxide-Cr₂O₃ compound(s) in the treated sarples calcined at 400 and 500 °C. Also, K₂O-doping conducted at 400 °C increased the degree of crystallinity and particle size of MgO phase and exerted opposite effects in the crystallinity and particle size of CuO phase. The doping process either with K₂O or Cr₂O₃ effected a measurable progressive decrease (42–53%) in the specific surface area of the investigated system subjected to heat treatment at 400 and 500 °C. However, the opposite effect was observed upon doping with 1 and 2 wt.% Cr₂O₃ followed by heating at 500 °C. The catalytic activity of the investigated system decreased by doping with K₂O. The addition of 6 wt.% effected a decrease of 78% and 68% in the value of the reaction rate constant per unit surface area for the catalytic reaction carried out at 30 °C (k_{30 °C}⁻) over the doped catalysts calcined at 400 and 500 °C, respectively. Cr₂O₃-doping on the other hand, much increased the catalytic activity of the treated samples and an increase of 106% and 80% in the value of k_{30 °C} was observed upon doping with 6 wt.% Cr₂O₃ for the solids calcined at 400 and 500 °C, respectively. The results were discussed in terms of creation of new in pairs and conversion of some active sites (surface CuO) into less active site (K₃Cu₅O₄).     

Laser raman spectroscopic studies of the surface oxides formed on iron chromium alloys at elevated temperatures

Binary iron-base alloys containing chromium additions of 3, 9, 12 and 18 % were oxidized in air at elevated temperatures. Laser Raman spectroscopy has been used to determine the chemical compounds of the oxides of these alloys. It is found that the oxides formed on Fe-3Cr alloy at various elevated temperatures consist mainly of iron. However, for Cr additions ≥12 %, the surface oxide formed at 400°C consists of αFe₂O₃, Fe₃O₄ and spinel phases. With increasing oxidation temperature up to 850°C, the oxide scale consists of Cr₂O₃ and spinel phases only.     

Consolidation of Cr3C2 doping WC–1TiN–5MgO micro–nano composites by two-step sintering

The effect of Cr₃C₂ additions on WC–1TiN–5MgO composites by two-step hot-pressing sintering (heated to 1750°C and then immediately cooled to 1575°C with a soaking time of 60?min under a sintering pressure of 50?MPa) was comprehensively investigated. The microstructure was characterized by means of scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), and X-ray diffractometry (XRD). Mechanical properties, such as hardness, transverse rupture strength, and fracture toughness, were measured. The experimental results show that no η-phase or brittle phases such as W₂C were formed, and excellent mechanical properties were achieved for 0.6?wt.% Cr₃C₂ additions with a hardness of 24.76?GPa, a flexural strength of 1257.1?MPa, and a fracture toughness of 10.08?MPa?·?mm^1/2. Cr₃C₂ addition brought about an improvement in the sinterability and contributed to the homogeneous distribution of second phase nanosized MgO. Crack deflection and crack bridging are the major mechanisms contributing to the drastically enhanced flexural strength and fracture toughness.     

Microstructural thermostability of high nitrogen austenitic stainless steel

A high nitrogen austenitic stainless steel, Fe–24Mn–18Cr–3Ni–0.62N, was isothermally annealed from 750 to 900 °C for different times to investigate the thermostability of its microstructures. Results show that the precipitates were Cr₂N and initially formed along the grain boundary. The time–temperature–precipitation diagram was established, according to which the critical cooling rate of this material with less than 0.1–0.5 vol.% of precipitated Cr₂N was specified as 30 °C/min. The microhardness of the matrix in samples annealed at different temperatures decreased with the diffusion of nitrogen from the matrix to grain boundaries.     

Formation of intermetallic phases during mechanical alloying and annealing of Cr + 20 wt % al mixtures

We have studied phase-formation processes in mixtures of Cr and Al (20 wt %) powders in the course of mechanical alloying (MA) and the phase transformations of the samples during subsequent annealing at temperatures of up to 800°C. The resultant x-ray amorphous intermetallic phases were identified by a differential dissolution method, which allows one to follow the formation of x-ray amorphous and partially crystallized phases. During MA of Cr + Al mixtures, the first to form is x-ray amorphous Cr₄Al, which then converts to partially crystallized Cr₂Al through reaction with aluminum. The peritectoid decomposition of Cr₄Al during heating of the MA samples is accompanied by heat release at 330–350°C. Heating to 420°C leads to the formation of Cr₅Al₈. At 800°C, Cr₅Al₈ reacts with Cr to form Cr₂Al.     

Microstructure stability and oxidation behaviour of (FeCoNiMo)90(Al/Cr)10 high-entropy alloys

Simple ordered L1₂ phase and complex ordered µ phase were found in the (FeCoNiMo)₉₀Al₁₀ alloy, while disordered FCC and µ phases were detected in the (FeCoNiMo)₉₀Cr₁₀ alloy. After annealing at 900°C, nano-size precipitates were observed in the L1₂ phase, and splitting and spheroidisation were occurred in some regions of the eutectic structures in the (FeCoNiMo)₉₀Cr₁₀ alloy. After holding for 100?h at 900°C, (FeCoNiMo)₉₀Al₁₀ alloy showed an excellent hardness resistance. The oxidation kinetics of both (FeCoNiMo)₉₀Al₁₀ and (FeCoNiMo)₉₀Cr₁₀ alloys followed a parabolic rate law at 900°C. An external layer of Al₂O₃ and an underlying MoO₂ subscale were found in the (FeCoNiMo)₉₀Al₁₀ alloy. A semi-continuous oxide layer of MoO₂ and Cr₂O₃ was observed in the (FeCoNiMo)₉₀Cr₁₀ alloy.     

Constitution and properties of ceramized fireclay refractories: I. Constitution

A poor-grade fireclay was mixed with three nucleating agents, namely Cr₂O₃, V₂O₅ and TiO₂. The fireclay and oxide mixed fireclay were fired at 1300°C for 1 h, cooled down to room temperature and then heat-treated at 1150°C for 15h. These were also heat-treated at 1150°C for 15 h after cooling down to 1150°C from the peak temperature. The heat-treatment caused ceramization of the glassy phase in the fireclay samples, and the samples, mineralogical composition and microstructure were investigated. Ceramization brought about significant changes in the microstructure only.     

Effect of mechanical milling on Ni–TiH2 powder alloy filler metal for brazing TiAl intermetallic alloy: The microstructure and joint's properties

A TiH₂–50 wt.% Ni powder alloy was mechanically milled in an argon gas atmosphere using milling times up to 480 min. A TiAl intermetallic alloy was joined by vacuum furnace brazing using the TiH₂–50 wt.% Ni powder alloy as the filler metal. The effect of mechanical milling on the microstructure and shear strength of the brazed joints was investigated. The results showed that the grains of TiH₂–50 wt.% Ni powder alloy were refined and the fusion temperature decreased after milling. A sound brazing seam was obtained when the sample was brazed at 1140 °C for 15 min using filler metal powder milled for 120 min. The interfacial zones of the specimens brazed with the milled filler powder were thinner and the shear strength of the joint was increased compared to specimens brazed with non-milled filler powder. A sample brazed at 1180 °C for 15 min using TiH₂–50 wt.% Ni powder alloy milled for 120 min exhibited the highest shear strength at both room and elevated temperatures.     

Microstructure and strength of high nitrogen steel joints brazed with Ni-Cr-B-Si filler

Brazing of high nitrogen austenitic stainless steels was carried out by using Ni-Cr-B-Si filler metal. The effects of brazing temperature (1020–1100°C) on the microstructure and shear strength of the joints were investigated. The results show that BN compounds with hexagonal structure are formed at the interface by the reaction of N from substrate and B from filler. The brittle Cr₅B₃ compounds with high microhardness are observed in the centre of brazing seam. The BN content increases and the Cr₅B₃ content decreases with the increase in brazing temperature. However, the content of BN compounds played a determinable role on the joint strength. The optimal shear strength of joints was 176.7?MPa when the joining temperature was 1020°C.     

Nickel-Molybdän-Sinterstähle für hochbeanspruchte Teile

Nickel-Molybdenum Sintered Steels for High Duty Parts . Fe-Ni-Mo steels without additions and with 0,45% P resp. 0,5% C added were sintered at 1150°C resp. 1250°C for 1 h in H₂. 2% Ni and 1,5% Mo resp. 4% Ni and 3% Mo were added as alloying elements. The strength of the sintered Fe-Ni-Mo alloys without additional elements did not exceed remarkably that of the sintered steels used up to now. Fe-Ni-Mo steels with 4% Ni and 3% Mo sintered at 1250°C with an addition of 0,45% P resp. 0,5% C have a tensile strength of 740 N/mm² resp; 830 N/mm². However the impact toughness of the alloy with P is remarkably higher than that of the alloy with C. The C-content determines mainly the strength properties of the alloys with C and influences the diffusion of the Mo too. The influence of the Ni and Mo on the properties of the alloys with P is more obvious. Alloys with 4% Ni and 3% Mo containing 0,45% P have good static and dynamic strength and therefore are capable for high duty parts.     

Microstructure, corrosion and mechanical properties of 304 stainless steel containing copper, silicon and nitrogen

The effects of 0.086–0.336% nitrogen additions on the microstructure, corrosion and mechanical properties of type 304 austenitic stainless steel (SS) containing 2% copper and 2–3% silicon were studied. This study was carried out using scanning electron microscope (SEM), potentiodynamic, weight loss, hardness number and ball-punch bulge measurements. Mutual effects between Si and N were observed in the matrix of SS. Nitrogen offset the ferrite-forming tendencies of Si and was more efficient than Ni as austenitizer, but Si decreased the solubility of N in solid solution. N additions improved the pitting resistance of SS in acidic and neutral chloride solutions. This was more evident in more aggressive solutions than in solutions with low chloride concentrations. Segregation of second N-rich phases, like Cr₂N, in SS containing 2% Cu, 3% Si and 0.237% N was occurred. This steel exhibited less pitting corrosion resistance than the plain 304 SS in most chloride solutions under study. Addition of 2% Si to 304 SS containing Cu has negative effect on the mechanical behavior. But presence of N improved the mechanical strength of steel irrespective of the drop solubility of N affected by Si.     

Microstructure and properties of SiC-whisker-reinforced Si<Subscript>3</Subscript>N<Subscript>4</Subscript> ceramics with calcium aluminate additions

Silicon-nitride-based ceramics containing Al₂O₃-CaO sintering aids and reinforced with silicon carbide whiskers have been prepared by hot pressing at 1650°C in a nitrogen atmosphere, and their microstructure, phase composition, and mechanical properties have been studied. The results indicate that the Si₃N₄ ceramic containing 15 wt % calcium aluminate additions and 10 wt % SiC fibers has a dense microstructure with a uniform distribution of skeletal and dendritic silicon carbide crystals. The observed variations in the morphology of the crystals are tentatively attributed to the secondary crystallization of silicon carbide from the eutectic calcium aluminate melt during cooling.     

Effect of annealing temperature on the microstructure and mechanical properties of an as-rolled Mg-9wt.%Li-3wt.%Al-1wt.%Zn alloy sheet

This study investigated the effect of annealing temperature on the mechanical properties of an as-rolled Mg-9.26wt.%Li-3,03wt,%Al-1,10wt.%Zn （LAZ931） alloy sheet. The dual-phase （a ＋ 13） LAZ931 alloy plate of 3 mm in thickness were roiled （67% reduction） and then annealed at temperatures at 100℃-350℃. The alloy＇s ductility showed a sharp concave downward tendency as a function of annealing temperature, The elongation of the LAZ931 alloy sheet increased with annealing temperature up to 150℃, followed by a sharp decrease of the alloy＇s ductility as the annealing temperature higher than 150℃. The specimen exhibited an extremely low elongation （only -0,5%） at annealing temperature around 300℃. Formation of brittle AILi particles on boundary resulted in Li depletion zone near by grain boundary, transforming the Li depletion zone into a （hcp） layer. The combined effects including brittle AILi particles on boundary and the hcp α layer on boundary resulted in the brittlement of the high-temperature-annealing sample.     

Thermal stability of heat-treated flame-synthesized anatase TiO<Subscript>2</Subscript> nanoparticles

In this article, TiO₂ nanoparticles were synthesized by using O₂-enriched coflow, hydrogen, diffusion flames. We investigated the thermal stability of the flame-synthesized TiO₂ nanoparticles by examining the crystalline structures of the nanoparticles and by analyzing the photocatalytic degradations of methylene blue solutions. Also, the results were compared with those of commercial P-25 nanoparticles. The maximum centerline temperature of the flame was measured to be 1,743 °C. Under this synthesis condition, TiO₂ nanoparticles, which were spherical with diameters approximately ranging from 30 to 60 nm, were synthesized. From the XRD analyses, about 96 wt.% of the synthesized nanoparticles were anatase-phase. After the heat-treatment at 800 °C for 30 min, the synthesized TiO₂ nanoparticles showed no significant changes of their shapes and crystalline phases. On the other hand, most of the commercial particles sintered with each other and changed to the rutile-phase. Whereas the photocatalytic ability of heat-treated commercial particles deteriorated, that of the flame-synthesized particles improved. On the basis of the improved result of photocatalytic degradation of methylene blue by using the heat-treated flame-synthesized nanoparticles, it is believed that the flame-synthesized TiO₂ nanoparticles have higher thermal stability at 800 °C than the commercial particles.     

Oxidation of electrodeposited black chrome selective solar absorber films

X-ray photoelectron spectroscopy and Auger electron spectroscopy were used to study the composition and oxidation of electrodeposited black chrome films. The outer layer of the film is Cr₂O₃ and the inner layer is a continuously changing mixture of chromium and Cr₂O₃. Initially, approximately 40 vol.% of the chromium was combined as Cr₂O₃ and the percentage of Cr₂O₃ increased to greater than 60 vol.% after heat treatment for only 136 h at 250°C. After 3600 h at 400°C the percentage of Cr₂O₃ increased to as high as 80 vol.%. The thermal emittance decreased approximately linearly with increasing oxide content whereas the solar absorptance remained constant until the percentage of Cr₂O₃ exceeded approximately 70%. Oxidation was slower when the Cr³⁺ concentration in the plating bath was reduced from 16 to 8 g 1^?1 and when black chrome was deposited on stainless steel rather than on sulfamate nickel.     

Effect of solid solution state of zirconium and Al3Zr (L12) precipitates on the recrystallization behavior of Al-0.2 wt.%Zr alloy

Effect of homogenization annealing on the existence form of zirconium in Al-0.2wt.%Zr alloy and effect of various existence form of zirconium on the recrystallization behavior of Al-0.2wt.%Zr cold-rolled (total deformation is 92.8 %) sheet are studied. The results show that large numbers of nearly spherical Al₃Zr (L1₂) nanoparticles precipitated from aluminum matrix after homogenizing at 475 °C for 24 h. Moreover, due to the precipitation of Al₃Zr particles, the hardness and electrical conductivity of the as-cast Al-0.2wt.%Zr alloy is increased from 25.1±0.5 HV 3 and 54.0±0.2 %IACS to 28.6±0.7 HV 3 and 56.2±0.1 %IACS, respectively. Hence, zirconium exists as solid solution state in the as-cast Al-0.2wt.%Zr alloy and metastable Al₃Zr phase in the homogenized alloy. Moreover, the recrystallization temperature of the pure aluminum without addition of zirconium is 300 °C, while the recrystallization temperature of the Al-0.2wt.%Zr alloy without and with homogenization is about 350 °C and 400 °C, respectively. Obviously, the solid solution state of zirconium has certain effect on retarding the recrystallization of aluminum alloy, while the nanometer Al₃Zr particles can inhibit the recrystallization of aluminum alloy effectively and increase the recrystallization temperature remarkably.     

Synthesis Pressure–Temperature Effect on Pinning in MgB2-Based Superconductors

The volume pinning force, F _p(max), increases with increasing synthesis or sintering pressure (0.1 MPa–2 GPa) in materials prepared at high temperature (1050 °C) while it stays practically unchanged in those prepared at low temperature (800 °C). The position of F _p(max) can be shifted to higher magnetic fields by: (1) increasing the manufacturing pressure or decreasing the temperature (2) additions (Ti, SiC, or C, for example), and (3) in-situ preparation. Grain boundary pinning (GBP) dominates in materials prepared at low temperatures (600–800 °C), while high-temperature preparation induces strong point pinning (PP) or mixed pinning (MP) leading to outstanding properties. In materials produced by spark plasma sintering (SPS), the position of F _p(max) is higher than expected for both grain boundary and point pinning. The distribution of boron and oxygen in MgB₂ based material, which can changed by additions or the preparation conditions, significantly affects the type and strength of pining. Materials prepared under a pressure of 2 GPa with a nominal composition of Mg:7B or Mg:12B consist of 88.5 wt % MgB₁₂, 2.5 wt % MgB₂, 9 wt % MgO or 53 wt % MgB₁₂, 31 wt % MgB₂₀ 16 wt % MgO, respectively. Their magnetic shielding fractions at low temperatures are 10 % and 1.5 %, with a transition temperature, T _c of 37.4–37.6 K. Although their magnetic critical current density at zero field and 20 K was 2–5×10² A/cm², they were found to be insulating on the macroscopic level.