High temperature fracture behavior of tungsten fiber reinforced copper matrix composites under dynamic compression

W_f/Cu₈₂Al₁₀Fe₄Ni₄ composite was fabricated by flow casting method. Dynamic compression tests with strain rate of 1600 s⁻¹ at 20 °C, 200 °C, 400 °C and 600 °C were finished by means of Split Hopkinson Pressure Bar (SHPB). The results showed that the composites possessed obvious high temperature softening behaviors. The damages of W_f/Cu₈₂Al₁₀Fe₄Ni₄ composites all occurred within the tungsten fibers when compressed at 20 °C, 200 °C and 400 °C, indicating that the interface strength of the composites was high. While the damages of the composites occurred either in the tungsten fibers or in the matrix at 600 °C, in addition, the melt of matrix alloy also occurred. Microstructure of the composites after dynamic compressing at 600 °C was analyzed by transmission electron microscope (TEM), observation revealed that there were a lot of high-density dislocations, stacking faults and twins existing in the matrix. It was also found that the precipitated phase in the matrix played the role of the second phase strengthening.     

Effect of filament temperature and deposition time on the formation of tungsten silicide with silane

The effect of filament temperature and deposition time on the formation of tungsten silicide upon exposure to the SiH₄ gas in a hot wire chemical vapor deposition process was studied using the techniques of cross-sectional scanning electron microscopy and Auger electron spectroscopy. At a relatively low temperature of 1500 °C, the decomposition of WSi₂ phase and the diffusion of Si towards the silicide/W interface produce a thick W₅Si₃ layer. The diffusional nature leads to a parabolic rate law for silicide growth. An exponential decrease of silicide thickness with temperature between 1600 and 2000 °C illustrates the dominance of Si evaporation at higher temperatures (T ≥ 1600 °C) over the silicide formation.     

Low-temperature plasma-enhanced chemical vapor deposition of tungsten and tungsten nitride

Tungsten and tungsten nitride layers have been deposited by plasma-enhanced chemical vapor deposition (PECVD). Tungsten layers deposited at low deposition temperatures T150 °C using this method showed good uniformity over dielectric and silicon substrate areas. As the deposition temperature decreased, the silicon consumed during the deposition reaction decreased, at T150 °C no silicon consumption was measurable. PECVD tungsten nitride layers were deposited directly on oxidized silicon substrates with no requirement for a nucleation layer. As the NH₃ flow rate was increased, whilst maintaining all other parameters constant, deposited layers were found to change from metal tungsten to tungsten-rich amorphous layer to W₂N. The resistivity of the layers was found to be high compared to published literature for higher-temperature deposited layers. The high resistivity is attributed to the incorporation of fluorine into the layer at low deposition temperatures. A deposition process was established for smooth amorphous tungsten-rich W _x N layers at 150 °C.     

Reactive sintering of boron-doped Ni76Al24 intermetallic

A preliminary investigation into the formation of boron-doped nickel-rich Ni₃Al with boron additions up to 2 wt% (i.e. to levels above the equilibrium solid solubility limit of boron in Ni₃Al) from elemental powders by reaction synthesis was carried out. The application of reaction synthesis was seen as a low-energy alternative to the production of Ni₃Al/boride composite suitable for wear applications. X-ray diffraction, Neutron diffraction, SEM/EDS,WDS, Image analysis, Archimedes principle and Rockwell hardness measurements; were used to study the effect of boron addition on the final microstructure, average grain size, bulk density and hardness of as-prepared Ni₇₆Al₂₄. Up to 0.3 wt% boron content, the microstructure consisted of single-phase Ni₃Al, however, at a boron content of 0.5 wt% an apparent transition from a single phase microstructure to a two-phase intermetallic/boride composite microstructure was observed, which dominated when the boron content increased, up to 2 wt%. The two-phase microstructure was identified as Ni₃Al (particles) within an Ni₄₁Al₅B₁₂ boride matrix, with no remaining un-reacted boron. The boron addition was found to increase the Rockwell hardness of Ni₃Al via two mechanisms. Below the solubility limit, the increase in hardness was due to solution hardening. Above 0.5 wt%B, solution hardening in addition to the formation of the harder boride phase, were found to amount to up to 50% increase in the hardness compared with boron free Ni₃Al. The extrusion of semi-molten beads at the surface of the compact at high B-content may be a limiting factor, in the formation of Ni₃Al/boride composites via this route.     

Solid-state synthesis of tungsten carbide from tungsten oxide and carbon, and its catalysis by nickel

Tungsten carbide has been produced by heating a mixture of tungsten oxide and carbon powder at 1300 °C for 2 h. Further batches were made with additional KCl, KCl + Ni, or KCl + Fe. The products were compared by XRD and SEM. A mixture of WC and W₂C was produced from the plain WO₃/carbon reaction, but adding 1 wt.% nickel assisted the formation of a pure WC phase. Both Ni and Fe assisted the growth of larger WC crystals.     

Reactive deposition of tungsten and titanium carbides by induction plasma

A study is reported on the use of induction plasma technology for the preparation of dense free-standing deposits of tungsten carbide and titanium carbide from metallic powders and methane. Phase analysis by X-ray diffraction indicates that primary carburization of the particles takes place in-flight giving rise to the formation of W₂C and TiC_1–x . Secondary carburization occurs in the deposits resulting in the formation of tungsten and titanium carbides. Microstructures revealed by optical and scanning electron microscopy show uniform small grains of the carbides. The reactive plasma spray-formed tungsten carbide shows transgranular fracture, while pure tungsten deposits show intergranular fracture.     

Assessment of B4C reaction with liquid iron alloys

The degree of reaction achieved when B₄C powders are brought into contact with liquid iron alloys has been assessed by a levitation dispersion test. Reaction occurs rapidly, leading to boron carbide dissolution and iron boride formation. In carbon-free iron alloys borocarbide, Fe₂₃(C, B)₆, also forms and in low-carbon iron alloys free graphite was also formed. Highcarbon alloys reacted to form both Fe₃(C, B) and free graphite. Attempts to provide protection for the B₄C by forming a TiC coating on its surface byin situ reactions with liquid Fe-Ti and Fe-Ti-C alloys proved unsuccessful, with TiC forming as a dispersed phase throughout the iron matrix     

Chemical reactivities of hafnium and its derived boride, carbide and nitride compounds at relatively mild temperature

MB₂/SiC composites are materials of choice for ultra-high-temperature structural applications, primarily in the aerospace arena. These composites are processed in a hot-press operation at a temperature range of 1900 to 2200°C. This article assesses potential mild-temperature (below 1500°C) chemical reactions that may lead to structures and coatings made of HfB₂/SiC under pressureless or mild-pressure conditions. The reactions are anticipated to be involved in reactive and shape-forming processes, where ceramic precursors and/or reactive powders are incorporated. This article pays special attention to exothermic reactions as well as to formers of a liquid phase; both can aid the desired phase formation, microstructure development, and sintering of the composite under milder conditions than currently practiced. Reactions between loosely mixed powders with melting points significantly above 1500°C were detected by X-ray diffraction (XRD) analyses. Significant solid-phase reactions of the loose powder mixtures were observed at this mild temperature in powder form. Preliminary microstructural studies using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray Spectroscopy (EDX) techniques have confirmed the presence of unique reaction mechanisms between the loosely connected particles.Good examples are the reactions between Hf powder and powders of BN or B₄C, all having melting points above 2200°C, which form at 1500°C, or below HfB₂/HfN and HfB₂/HfC crystalline domains, respectively. These reactions are less intuitive than the reaction with B₂O₃, which forms HfB₂/HfO₂, potentially via molten or gaseous phases of boron oxide.     

The effects of substrate bias on phase stability and properties of sputter-deposited tungsten carbide

The effects of substrate bias on phase formation and physical properties of rf magnetron sputter-deposited tungsten carbide films have been investigated in this work. Films were deposited at 275 °C using bias levels ranging from 0 to −150 V and at room temperature and −160 V. At low bias levels, the films were primarily composed of the WC_1−x/W₂(C,O) phases, both of which have the B1 structure, and the fraction of the hexagonal W₂C phase increased with bias level. The increased substrate bias levels also correlated with a reduction in oxygen content, suggesting that reducing oxygen content promotes formation of the W₂C phase. However, the film deposited at room temperature and −160 V bias had an oxygen content of only 3%, yet did not form the W₂C phase, indicating a minimum level of thermal activation is also required to form W₂C. Increasing the bias voltage also resulting in increases in film hardness, modulus and compressive residual stress, while reducing resistivity.     

Mechanical alloying and sintering of nanostructured tungsten carbide-reinforced copper composite and its characterization

Elemental powders of copper (Cu), tungsten (W) and graphite (C) were mechanically alloyed in a planetary ball mill with different milling durations (0–60 h), compacted and sintered in order to precipitate hard tungsten carbide particles into a copper matrix. Both powder and sintered composite were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) and assessed for hardness and electrical conductivity to investigate the effects of milling time on formation of nanostructured Cu–WC composite and its properties. No carbide peak was detected in the powder mixtures after milling. Carbide WC and W₂C phases were precipitated only in the sintered composite. The formation of WC began with longer milling times, after W₂C formation. Prolonged milling time decreased the crystallite size as well as the internal strain of Cu. Hardness of the composite was enhanced but electrical conductivity reduced with increasing milling time.     

A comparative study of borided pure niobium, tungsten and chromium

Pure niobium (Nb), tungsten (W) and chromium (Cr) were boronized at 940 °C for 2, 4 and 8 h. The borided samples were characterized by X-ray diffraction, Scanning electron microscope and microhardness tests. Tribological investigation was conducted. X-ray study showed the presence of NbB₂, WB, and CrB. The hardnesses of boride layers formed on the pure Nb, W and Cr were 2500, 2500 and 1700 HV, respectively, whereas the hardnesses of the pure Nb, pure W and pure Cr were 110, 445 and 115 HV, respectively. Nb boride layers ranged in thickness from 8 to 22 μm, whereas W boride layers ranged in thickness from 10 to 42 μm, and the thickness of Cr boride layer varied from 4 to 12 μm with boronizing time. The boriding of W resulted in thicker boride layer compared to the boriding of Nb and Cr at given time. The frictional behaviour and wear mechanicms differ in modes and scales.     

Synthesis of Fe based ZrB2 composite coating by gas tungsten arc welding

Abstract

ZrB₂/Fe composite coating was in situ synthesised by gas tungsten arc welding cladding process on AISI 1020 steel. Zr, B₄C and Fe–B alloy powders were used as precursor powders. The phase composition and microstructure were investigated by X-ray diffraction analysis, optical microscopy, scanning electron microscopy and energy dispersive spectroscopy. Microhardness of ZrB₂/Fe composite coating at room temperature was examined. Main phases obtained from Zr and B₄C precursor are ZrB₂ and α-Fe, and those obtained from Zr and Fe–B precursor are ZrB₂ and FeB. In the upper part of these composite coatings, ZrB₂ phase mainly grows along temperature gradient direction. The middle part of these composite coatings has the highest ZrB₂ content and highest microhardness. Gradient dispersions of ZrB₂ reinforcements appeared in the composite coating from the middle to the bottom, leading to gradient dispersions of microhardness. With decreasing dilution rate, ZrB₂ content and microhardeness increase.     

Kinetics of tungsten carbidization under non-isothermal conditions

Kinetic laws of high-temperature interaction between tungsten and methane are studied under non-isothermal conditions in the temperature interval 1273-2873 K. Computer Assisted Electrothermography was applied during which thin metallic wires 100 μm in diameter were directly heated up by electric current in the carbon-containing atmosphere. Experimental data on weight gain, carbide layer growth, and microstructure of phases are obtained in the linear heating regime at heating rates from 10 to 1500 K/s. We established that the interaction between tungsten and methane in a wide interval of pressure and heating rates may proceed with simultaneous or consecutive formation of W₂C and WC carbide phases. Experimental data on weight gain and carbide layer growth were processed using calculation schemes deduced within the framework of a reaction diffusion model with the first type boundary conditions under non-isothermal conditions. Kinetic and diffusion constants are determined for tungsten carbidization with formation of the W₂C phase.     

Effects of process parameters on tungsten boride production from WO3 by self propagating high temperature synthesis

In the present study, the production parameters of tungsten boride compounds by self-propagating high-temperature synthesis (SHS) method and following leaching process were investigated. In the SHS stage, the products consisting of tungsten borides, magnesium oxide, magnesium borate, and also minor compounds were obtained by using different initial molar ratios of WO₃, Mg and B₂O₃ as starting materials. In the leaching step, Mg containing byproducts, i.e. MgO and Mg₃B₂O₆, existed in the selected SHS product synthesized at 1:8:2.5 initial molar ratio of WO₃:Mg:B₂O₃ were leached out by using aqueous HCl solution to obtain clean tungsten boride compounds at different experimental parameters which are time, acid concentration and temperature. The acid leaching experiments of the SHS product showed that optimum leaching conditions could be achieved by using 5.8 M HCl at 1/10 S/L ratio and the temperature of 80 °C for 60 min.     

SiC matrix composites containing transition metal boride particulates internally synthesised by carbothermal reaction

SiC matrix composites reinforced with the various borides of the transition metals in group IV a-VI a, which were synthesized from the transition metal oxide, boron carbide and carbon mixed with SiC powder. Dense composites containing boride particulates of titanium, zirconium, niobium and chromium were prepared through reactive hot-pressing. The morphology of the internally synthesized boride particles reflected that of the starting oxide powders. SiC-NbB₂ composites with four-point flexural strength of 500 to 600 MPa and better oxidation resistance than SiC-TiB₂ were prepared even through pressureless sintering process. Pressureless-sintered and HIPed SiC-20 vol% NbB₂ exhibited the four-point flexural strength of 760 MPa at 20 °C and 820 MPa at 1400 °C.     

Electrical properties of vanadium tungsten oxide thin films

The vanadium tungsten oxide thin films deposited on Pt/Ti/SiO₂/Si substrates by RF sputtering exhibited good TCR and dielectric properties. The dependence of crystallization and electrical properties are related to the grain size of V_1.85W_0.15O₅ thin films with different annealing temperatures. It was found that the dielectric properties and TCR properties of V_1.85W_0.15O₅ thin films were strongly dependent upon the annealing temperature. The dielectric constants of the V_1.85W_0.15O₅ thin films annealed at 400 °C were 44, with a dielectric loss of 0.83%. The TCR values of the V_1.85W_0.15O₅ thin films annealed at 400 °C were about −3.45%/K.     

Synthesis of TiB2 powder from a mixture of TiN and amorphous boron

TiB₂ powder was synthesized by solid state reaction using amorphous boron and TiN as a source of titanium. The TiB₂ formation did not occur at all in a nitrogen atmosphere even at 1400° C. TiB₂ formed above 1100° C in argon and hydrogen atmospheres. The only crystalline phase of TiB₂ powder was favourably synthesized at 1400° C for 360 min in an argon atmosphere from a starting powder with a composition containing excess boron (B/Ti = 2.2). The synthesized powder was well dispersed and had a particle size of 0.5 to 2 µm. The powder activity was evaluated by sintering at 4 G Pa and 1300 to 1600° C for 15 min.     

The effect of boron on the microstructure and physical properties of chemically vapour deposited nickel films

The solid solution addition of boron greatly enhances the strength and hardness of chemically vapour deposited (CVD) nickel while dramatically changing the microstructure. The solid solubility of boron in nickel is limited, and single-phase alloys containing in excess of 0.3 at% B are supersaturated with respect to the formation of one or more intermetallic boride phases. Single-phase Ni-B alloys containing 0 to 13.0 at% B were produced by CVD on polycrystalline copper substrates at 155° C in an atmospheric pressure process. The microstructure, mechanical and physical properties were characterized for the alloys both as-deposited and after various thermal treatments by using optical microscopy, transmission electron microscopy, X-ray diffraction and micro-indentation hardness testing with a diamond pyramid indentor. The grain size of the alloy was found to decrease sharply with rising boron content. Concomitantly, the defect density of the material rose significantly, the microhardness increased and the ductility decreased. With annealing at a temperature of 300° C or greater, precipitation of the Ni₃B intermetallic phase, recovery and grain growth occurred.     

Precipitation of W2B5 and β-WB from Ti0.3W0.4Cr0.3B2 solid solutions

We investigated the formation of W₂B₅ and β-WB precipitates in supersaturated Ti_0.3W_0.4Cr_0.3B₂ solid solutions during isothermal annealing at temperatures between 1400 and 1600 °C. X-ray diffractometry measurements showed that the precipitation process is very complex including metastable phase formation and mutual transformation between the two precipitation phases. The rate constants of precipitation are determined as a function of reciprocal temperature and discussed in framework to literature data.     

Pressureless-sintered and HIPed SiC-TiB2 composites from SiC-TiO2-B4C-C powder compacts

Dense SiC-TiB₂ composites with prescribed compositions were obtained through pressureless sintering of SiC-TiO₂-B₄C-C powder compacts. During the process, TiO₂, B₄C and C reacted to form TiB₂, followed by the consolidation of SiC matrix with the aid of excess B₄C and C. The effects of the composition of the starting powders on the final density were investigated and the mechanical properties of the composite were evaluated. The sintered body with additional HIPing at 1900 °C exhibited the average four-point flexural strength of more than 700 MPa at both 20 and 1400 °C.