Effect of Nb content on the phase composition,densification, microstructure,and mechanical properties of high-entropy boride ceramics

Dense high-entropy (Hf,Zr,Ti,Ta,Nb)B₂ ceramics with Nb contents ranging from 0 to 20 at% were produced by a two-step spark plasma sintering process. X-ray diffraction indicated that a single-phase with hexagonal structure was detected in the composition without Nb. In contrast, two phases with the same hexagonal structure, but slightly different lattice parameters were present in compositions containing Nb. The addition of Nb resulted in the presence of a Nb-rich second phase and the amount of the second phase increased as the Nb content increased. The relative densities were all >99.5 %, but decreased from ～100 % to ～99.5 % as the Nb content increased from 0 to 20 at%. The average grain size decreased from 13.9 ± 5.5 μm for the composition without Nb additions to 5.2 ± 2.0 μm for the composition containing 20 at% Nb. The reduction of grain size with increasing Nb content was due to the suppression of grain growth by the Nb-rich second phase. The addition of Nb increased Young’s modulus and Vickers hardness, but decreased shear modulus. While some Nb dissolved into the main phase, a Nb-rich second phase was formed in all Nb-containing compositions.     

Effects of SiC content on the densification,microstructure, and mechanical properties of HfB2–SiC composites

To investigate the effects of SiC on microstructure, hardness, and fracture toughness, 0, 10, 20, and 30 vol% SiC were added to HfB₂ and sintered by SPS. Upon adding SiC to 30 vol%, relative density increased about 4%; but HfB₂ grain growth had a minimum at 20 vol% SiC. This may be due to grain boundary silicate glass, responsible for surface oxide wash out, enriched in SiO₂ with higher fraction of SiC. By SiO₂ enrichment, the glass viscosity increased and higher HfO₂ remained unsolved which subsequently lead to higher grain growth. Hardness has increased from about 13 to 15 GPa by SiC introduction with no sensible variation with SiC increase. Residual stress measurements by Rietveld method indicated high levels of tensile residual stresses in the HfB₂ Matrix. Despite the peak residual stress value at 20 vol% SiC, fracture toughness of this sample was the highest (6.43 MPa m^0.5) which implied that fracture toughness is mainly a grain size function. Tracking crack trajectory showed a mainly trans-granular fracture, but grain boundaries imposed a partial deflection on the crack pathway. SiC had a higher percentage in fracture surface images than the cross-section which implied a weak crack deflection.     

Role of MgO on densification and mechanical properties in spark plasma sintered Os0.9Re0.1B2 ceramic

To promote the densification and therefore the mechanical properties of boride-based ceramics, MgO was added as sintering aid into Os_0.9Re_0.1B₂ powders for densification by using spark plasma sintering (SPS). The Os_0.9Re_0.1B₂ powders were synthesized by mechanochemical method from powder mixture of Os, Re and amorphous B. The role of MgO on densification, phase composition, microstructure and mechanical properties (hardness, fracture toughness and wear behavior) were studied by using X-ray diffraction (XRD), scanning electron microscope (SEM) with energy-dispersive spectroscopy (EDS), micro indentation and ball-on-disk tribometer. The results show that, with the introduction of MgO as sintering aid, the relative density of the Os_0.9Re_0.1B₂ ceramic samples increased. When the MgO content reached 9 wt%, the as-sintered sample is almost fully dense. No obvious regularity was found from the samples with the addition of different content of MgO. Vickers hardness values of the samples with 0, 3 wt% and 9 wt% MgO are found to be very close with each other within the experimental error (~30 GPa), while the sample with the addition of 6 wt% MgO exhibits the highest hardness of ~35 GPa. The fracture toughness of the samples is decreased slightly with the addition of MgO. The friction coefficient and wear rate of the sample with the addition of 6 wt% MgO was also found to be the lowest among all samples, which indicate best wear resistance. As a whole, with the addition content of 6 wt% MgO, the Os_0.9Re_0.1B₂ ceramic sample performs relatively excellent mechanical properties among four groups of samples.     

A facile pathway to prepare molybdenum boride powder from molybdenum and boron carbide

Molybdenum boride is an ideal hard and wear-resistant material. In this study, a new method is proposed for preparing molybdenum boride, by which Mo first reacts with B₄C to generate the mixture of molybdenum boride and C, and then the product is decarburized by molten Ca to generate CaC₂. Pure molybdenum boride could be obtained after acid leaching to remove the by-product CaC₂. According to the experimental and thermodynamic calculation results, it is concluded that the single-phase MoB could be successfully prepared, while Mo₂B, Mo₂B₅, and MoB₄ could not be synthesized by this method. Moreover, it was found that the particle size of finally prepared MoB is determined by particle size of raw Mo powder. The residual carbon content of the product could be decreased to 0.10 wt% after first reaction at 1673 K for 6 hours and then decarburization reaction at 1673 K for 6 hours.     

High-entropy boride–carbide ceramics by sequential boro/carbothermal synthesis

A dual-phase high-entropy boride (HEB)/carbide (HEC) ceramic with a fine grain size was synthesized by a sequential boro/carbothermal process. In the first step, an Hf–Nb–Ta–Ti–Zr-containing carbide was synthesized by a carbothermal reduction of oxides followed by the reaction of the carbide with B₄C and ZrH₂ to convert part of the carbide to boride. The resulting composition was ∼29 vol% HEB with an average grain size of ∼1.1 μm. Solid solution formation occurred at the densification temperature of 1900°C resulting in a relative density higher than 99%. The Vickers hardness was 26.5 ± 1.4 GPa. This is the first report of synthesizing dual-phase boride–carbide high-entropy ceramics from carbothermally synthesized, HEC powders.     

Friction and Wear Behavior of Single-Phase Fe2B Bulk under Dry Sliding Condition

The effects of normal load and velocity on the friction and wear behavior of single-phase Fe₂B bulk have been investigated by optical microscopy, X-ray diffraction, scanning electron microscopy, and X-ray photoelectron spectroscopy. Results indicate that the friction coefficient and wear rate both decrease at first and then increase with increasing load and velocity, respectively. Attributed to the formation of a lamellar film on the Fe₂B surface, the lowest friction coefficient and wear rate are obtained at a velocity of 0.2 m/s under a load of 12 N. The dynamic friction coefficients under loads of 4 and 12 N are around 0.8 in the initial steady stage and then decrease to about 0.6, whereas the friction coefficient at 20 N shows no obvious change and remains around 0.82. The lubricating film consisting of Fe₂O₃, B₂O₃, SiO₂, and H₃BO₃ reduces the friction coefficient at 0.2 m/s under a load of 12 N.     

Pack boronizing of AISI H11 tool steel: Role of surface mechanical attrition treatment

The role of surface mechanical attrition treatment (SMAT) on pack boronizing of AISI H11 type tool steel is addressed. SMAT induced plastic deformation, enabled nanocrystallization at the surface, reduced the grain size and increased the volume fraction of non-equilibrium gain boundaries, increased the accumulation of defects and dislocations at the grain boundaries and within the grains. These features helped to promote the diffusion of boron during boronizing and increased the case depth and hardness of the borided layer. Duplex treatment on SMATed H11 steel samples helps to achieve a higher case depth when compared to the single stage treatment. The findings of the study suggest that SMAT can be used as a pre-treatment for boronizing of H11 tool steel.     

硼对等离子熔覆耐磨复合板的组织性能影响

采用等离子表面熔覆技术,在Q235基体钢板上熔覆无硼以及含硼（其它粉末成分不变）的铁基合金涂层。利用光学显微镜（OM）、扫描电镜（SEM）、X射线衍射仪（XRD）、电子探针（EMPA）、显微硬度计对涂层的组织、相组成和显微硬度等进行分析。结果表明,含硼粉末熔覆涂层含有（Fe,Cr）7（C,B）3等硼化物相,含量比无硼粉末涂层的（Fe,Cr）7C3等碳化物相含量明显增多;并且产生了大量的共晶硼化物FeB以及少量的Fe2B,均匀弥散的分布在涂层中;在α-Fe中也有间隙固溶的硼;且随着粉末成分含硼量的增加,（Fe,Cr）7（C,B）3硼化物相含量增多,熔覆涂层的平均和最高显微硬度值也相应增加。     

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.