Densification of SiO2–cBN composites by using Ni nanoparticle and SiO2 nanolayer coated cBN powder

Cubic boron nitride (cBN) powder was coated with Ni nanoparticle and SiO₂ nanolayer (abbreviated as cBN/Ni and cBN/SiO₂, respectively) by rotary chemical vapor deposition (RCVD), and compacted with SiO₂ powder by spark plasma sintering at 1473–1973 K for 0.6 ks. The effects of Ni and SiO₂ coatings on the densification, phase transformation of cBN and hardness of SiO₂–cBN composites were compared. The phase transformation of cBN to hBN was identified at 1973 K in SiO₂–cBN/SiO₂ composites, 300 K higher than that in SiO₂–cBN/Ni composites, indicating that SiO₂ retarded the transformation of cBN. The relative density of SiO₂–cBN/SiO₂ with 50 vol% cBN sintered at 1873 K was 99% with a hardness of 14.5 GPa.     

Consolidation of cubic and hexagonal boron nitride composites

Consolidating cubic boron nitride (cBN) typically requires either a matrix of metal bearing materials that are undesirable for certain applications, or very high pressures within the cBN phase stability field that are prohibitive to manufacturing size and cost. We present new methodology for consolidating high stiffness cBN composites within a hexagonal boron nitride (hBN) matrix (15–25 vol%) with the aid of a binder phase (0–6 vol%) at moderate pressures (0.5–1.0 GPa) and temperatures (900–1300 °C). The composites are demonstrated to be highly tailorable with a range of compositions and resulting physical/mechanical properties. Ultrasonic measurements indicate that in some cases these composites have elastic mechanical properties that exceed those of the highest strength steel alloys. Two methods were identified to prevent phase transformation of the metastable cBN phase into hBN during consolidation: 1. removal of hydrocarbons, and 2. increased cBN particle size. Lithium tetraborate worked better as a binder than boron oxide, aiding consolidation without enhancing cBN to hBN phase transformation kinetics. These powder mixtures consolidated within error of their full theoretical mass densities at 1 GPa, and had only slightly lower densities at 0.5 GPa. This shows potential for consolidation of these composites into larger parts, in a variety of shapes, at even lower pressures using more conventional manufacturing methods, such as hot-pressing.     

Densification and mechanical properties of cBN–TiN–TiB2 composites prepared by spark plasma sintering of SiO2-coated cBN powder

cBN–TiN–TiB₂ composites were fabricated by spark plasma sintering at 1773–1973 K using cubic boron nitride (cBN) and SiO₂-coated cBN (cBN(SiO₂)) powders. The effect of SiO₂ coating, cBN content and sintering temperature on the phase composition, densification and mechanical properties of the composites was investigated. SiO₂ coating on cBN powder retarded the phase transformation of cBN in the composites up to 1873 K and facilitated viscous sintering that promoted the densification of the composites. Sintering at 1873 K, without the SiO₂ coating, caused the relative density and Vickers hardness of the composite to linearly decrease from 96.2% to 79.8% and from 25.3 to 4.4 GPa, respectively, whereas the cBN(SiO₂)–TiN–TiB₂ composites maintained high relative density (91.0–96.2%) and Vickers hardness (17.9–21.0 GPa) up to 50 vol% cBN. The cBN(SiO₂)–TiN–TiB₂ composites had high thermal conductivity (60 W m⁻¹ K⁻¹ at room temperature) comparable to the TiN–TiB₂ binary composite.     

Influence of hBN content on mechanical and tribological properties of Si3N4/BN ceramic composites

Silicon nitride materials containing 1–5 wt% of hexagonal boron nitride (micro-sized or nano-sized) were prepared by hot-isostatic pressing at 1700 °C for 3 h. Effect of hBN content on microstructure, mechanical and tribological properties has been investigated. As expected, the increase of hBN content resulted in a sharp decrease of hardness, elastic modulus and bending strength of Si₃N₄/BN composites. In addition, the fracture toughness of Si₃N₄/micro BN composites was enhanced comparing to monolithic Si₃N₄ because of toughening mechanisms in the form of crack deflection, crack branching and pullout of large BN platelets. The friction coefficient was not influenced by BN addition to Si₃N₄/BN ceramics. An improvement of wear resistance (one order of magnitude) was observed when the micro hBN powder was added to Si₃N₄ matrix. Mechanical wear (micro-failure) and humidity-driven tribochemical reaction were found as main wear mechanisms in all studied materials.     

Reactive sintering cBN-Ti-Al composites by spark plasma sintering

When synthesizing polycrystalline cubic boron nitride (PcBN) at normal pressure, cBN had a trend of hexagonal transformation, which reduces the hardness and strength of PcBN. The cBN-Ti-Al composite was prepared by spark plasma sintering with introducing Ti and Al to absorb hexagonal boron nitride (hBN) transformed from cBN. By the results of X-ray diffraction (XRD), Ti and Al reacted with BN and forming TiN, TiB₂, and AlN, which combined cBN as the binder by chemical bonding. The mechanical properties of the prepared composite increased as the increment of sintering temperature. The threshold temperature for preparing composite without hBN phase was at 1400 °C. The composite with optimal mechanical properties was prepared at 1400 °C, and the relative density, the bending strength, hardness, and fracture toughness were 98.9 ± 0.1%, 390.7 ± 4.4 MPa, 14.1 ± 0.5 GPa, and 7.6 ± 0.1 MPa·m^0.5, respectively.     

Synthesis and characterization of novel Ti3SiC2–cBN composites

In this paper, synthesis of novel super hard and high performance composites of titanium silicon carbide–cubic boron nitride (Ti₃SiC₂–cBN) was evaluated at three different conditions: (a) high pressure synthesis at ~ 4.5 GPa, (b) hot pressing at ~ 35 MPa, and (c) sintering under ambient pressure (0.1 MPa) in a tube furnace. From the analysis of experimental results, the authors report that the novel Ti₃SiC₂–cBN composites can be successfully fabricated at 1050 °C under a pressure of ~ 4.5 GPa from the mixture of Ti₃SiC₂ powders and cBN powders. The subsequent analysis of the microstructure and hardness studies indicates that these composites are promising candidates for super hard materials.     

Mechanical properties of nano-polycrystalline cBN synthesized by direct conversion sintering under HPHT

Using hBN and pBN as starting materials, various types of binderless polycrystalline cBN (BL-PcBN) were synthesized in the pressure range of 8–20 GPa and temperature range of 1300–2400 °C, and their mechanical properties were evaluated. In the synthesis pressure range of 10 GPa and higher, the hardness of BL-PcBN showed a correlation not with the synthesis pressure, but with the synthesis temperature. Binderless polycrystalline cBN synthesized at about 2200 °C exhibited the highest mechanical properties, for both starting materials. Specifically, BL-PcBN(h) (100–300 nm grain size) synthesized from hBN at 10 GPa and 2200 °C showed a hardness of 45 GPa, transverse rupture strength of 1.6 GPa. In contrast, BL-PcBN(p) synthesized from pBN at the same temperature had finer grain size (50–100 nm) and exhibited the same level of hardness but lower strength properties (transverse rupture strength of approx. 1.3 GPa) than BL-PcBN(h). Consequently, the material that exhibited the best mechanical properties was BL-PcBN(h) synthesized at 10 GPa and 2200 °C. A prototype micro ball end mill made of this material was examined in a mirror-like (polished-like) finishing test using high-strength hardened steel. This ball end mill achieved a fine finishing surface with a surface roughness (Ra) of 20 nm or better. The test revealed the high potential of this material for use as a high-precision cutting tool for high strength ferrous materials.     

Effects of additive LiF on the synthesis of cBN in the system of Li3N–hBN at HPHT

High-quality cBN single crystals were successfully synthesized in the system of Li₃N–hBN with additive LiF at high pressure and high temperature (HPHT). The lowest synthetic conditions of cBN decreased to 4.6 GPa, 1320 °C by employing 3 wt.% LiF, and it didn't change anymore though more than 3 wt.% LiF had been added. The quality of cBN crystals improved markedly. The cBN crystals and other products were examined by X-Ray diffraction and scanning electron microscopy. The X-Ray analysis reveals that the “graphitization index” (GI) of hBN increased by adding 3 wt.% LiF into the system of Li₃N–hBN at HPHT. The SEM photographs show that different growth steps were formed on the cBN crystal surface in systems of Li₃N–hBN and Li₃N–LiF–hBN, respectively.     

Microstructure and tribological properties of cubic boron nitride films on Si3N4 inserts via boron-doped diamond buffer layers

Cubic boron nitride (cBN) coatings were deposited on silicon nitride (Si₃N₄) cutting inserts through conductive boron-doped diamond (BDD) buffer layers in an electron cyclotron resonance microwave plasma chemical vapor deposition (ECR MPCVD) system. The adhesion and crystallinity of cBN coatings were systematically characterized, and the influence of doping level of BDD on the phase composition and microstructure of the cBN coatings were studied. The nano-indentation tests showed that the hardness and elastic modulus of the obtained cBN coatings were 78 GPa and 732 GPa, respectively. The tribological properties of the cBN coatings were evaluated by using a ball-on-disc tribometer with Si₃N₄ as the counterpart. The coefficient of the friction and the wear rate of the cBN coatings were estimated to be about 0.17 and 4.1 × 10^− 7 mm³/N m, respectively, which are remarkably lower than those of titanium aluminum nitride (TiAlN) coatings widely used in machining ferrous metal. The results suggest that cBN/BDD coated Si₃N₄ inserts may have great potentials for advanced materials machining.     

cBN reinforced Y-α-SiAlON composites

Dense α-Sialon–cBN composites were produced by FAST/SPS–sintering at 1575–1625 °C. The hardness of the materials increases only up to 21 GPa for materials with 10 vol.% cBN. On the other hand the fracture toughness increases up to nearly 8 MPa m^0.5 with 30 vol.% cBN. The reason for the increase in fracture toughness is attributed to crack deflection at cBN grains due to the weak bonding of the grains in the matrix. The weak interfaces are also responsible for the moderate increase in hardness. Detailed investigation of the interface between cBN and the matrix was carried out by TEM.     

Elastic properties of translucent polycrystalline cubic boron nitride as characterized by the dynamic resonance method

Cubic boron nitride (cBN) is second only to diamond in a number of extreme material properties, and its performance exceeds diamond in many applications involving contact with ferrous alloys and/or high temperatures. However, its properties are less well understood. We have sintered cBN powder (2–4 μm or 8–12 μm particle size) into pure, translucent, polycrystalline compacts by pressing at a pressure of 7.7 GPa and temperatures from 2100 to 2350°C without any sintering agent. We have determined the Young's modulus E, shear modulus G, and Poisson's ratio ν of a number of translucent polycrystalline cBN compacts, in the form of free-standing disks, using the dynamic resonance method. The measured values for E, G, and ν lay in the ranges of 665–895 GPa, 295–405 GPa, and 0.11–0.15, respectively, depending on the grain size of the cBN starting material and the sintering temperature. These values may be compared with the theoretical values of E, G, and ν for pure, equiaxed, cBN of 909 GPa, 405 GPa, and 0.12, respectively. Combining the Young's modulus with previous Vickers hardness measurements, the fracture toughness K_IC of well-sintered translucent PCBN is evaluated as 6.8 MPa m^1/2. The dependence of the elastic properties on the synthesis conditions is discussed in the context of the microstructure and of related material properties.     

Microstructure,hardness and fracture toughness of spark plasma sintered ZrB2–SiC–Cf composites

The combined effects of SiC particles and chopped carbon fibers (C_f) as well as sintering conditions on the microstructure and mechanical properties of spark plasma sintered ZrB₂-based composites were investigated by Taguchi methodology. Analysis of variance was used to optimize the spark plasma sintering variables (temperature, time and pressure) and the composition (SiC/C_f ratio) in order to enhance the hardness of ZrB₂–SiC–C_f composites. The sintering temperature was found as the most effective variable, with a significance of 83%, on the hardness. The hardest ZrB₂-based ceramic was achievable by adding 20 vol% SiC and 10 vol% C_f after spark plasma sintering at 1850 °C for 6 min under 30 MPa. Fracture toughness improvement were related to the simultaneous presence of SiC and C_f phases as well as the in-situ formation of nano-sized interfacial ZrC particles. Crack deflection, crack branching and crack bridging were detected as the toughening mechanisms. A Vickers hardness of 14.8 GPa and an indentation fracture toughness of 6.8 MPa m^1/2 were measured for the sample fabricated at optimal processing conditions.     

Microstructure and mechanical properties of yttria stabilized zirconia coatings prepared by plasma spray physical vapor deposition

Plasma spray physical vapor deposition (PS-PVD) was used to deposit yttria stabilized zirconia (YSZ) coatings with different columnar morphologies by varying the spray distance. Although similar quasi-columnar structures were formed at the spray distances of 600 mm and 1400 mm, the formation mechanisms of particles in the coatings were different. Besides, an electron beam physical vapor deposition (EB-PVD) like columnar coating out of pure vapor was deposited at a spray distance of 1000 mm and the columnar consisted of elongated nano-sized secondary columns. The hardness and Young׳s modulus of the coatings were investigated. Compared to the other two quasi-columnar structures, the EB-PVD like columnar coating exhibited higher hardness (~9.0 GPa ) and Young׳s modulus (~110.9 GPa), mainly due to its low porosity and defect.     

Al2O3-3YTZP-Graphene multilayers produced by tape casting and spark plasma sintering

This work aims to establish a colloidal route to obtain laminates of alumina–zirconia combining layers with and without graphene. Green tapes of alumina, alumina with 5 vol.% of 3Y-TZP and alumina with 5 vol.% of 3Y-TZP and graphene-oxide (2 vol.%) were obtained by aqueous tape casting. It is possible to design materials for different structural applications with a controlled microstructure with a high number of different layers. The tapes were punched into 20-mm discs, joined to form laminates alternating up to 18-layers, and sintered in one-step by spark plasma sintering (SPS) at 1400 °C. It has demonstrated that there is a significant graphite diffusion provoked by the required graphite holders into the SPS-furnace. Dense laminates with layer thicknesses ∼100 μm and good cohesion between layers were obtained. Nanoindentation results showed that hardness and elastic modulus values were higher than 27 GPa and 300 GPa, respectively, and similar for all layers.     

Microstructure and mechanical properties of hot pressed Al2O3/SiC nanocomposites

Al₂O₃/SiC micro/nano composites containing different volume fractions (5, 10, 15, and 20 vol.%) of SiC were prepared by mixing a sub-micron alumina powder with respective amounts of either micro- or nano-sized silicon carbide powders. The powder mixtures were hot pressed 1 h at 1740 °C and 30 MPa in the atmosphere of Ar. The effect of SiC addition on the microstructure and mechanical properties, i.e. hardness, fracture toughness, and room temperature flexural strength were investigated. The flexural strength increased with increasing volume fraction of silicon carbide particles. The maximum flexural strength (655 ± 90 MPa) was achieved for the composite containing 20 vol.% of coarse-grained SiC, which is more than twice as high as in the Al₂O₃ reference. Hardness and fracture toughness were also moderately improved. The observed improvement of mechanical properties is mainly attributed to alumina matrix grain refinement and grain boundary reinforcement.     

Net shape forming of green alumina via CNC machining using diamond embedded tool

Diamond embedded tools were fabricated through nickel electroplating of mild steel conical shaped shank for machining of green alumina compacts using Computer Numerical Control (CNC) machine. Flat and pointed end conical tools embedded with different grain sizes viz. ～117 μm (120 mesh) and ～20 μm (625 mesh) of diamond particles were used for green machining of alumina. The hardness values of 625 and 120 mesh tools were measured to be 13.79±3 GPa and 11.84±6 GPa, respectively. Diamond embedded tools were successfully used for net shape fabrication of symmetrical and unsymmetrical objects such as cylinder, dental crown, 3D pattern via CNC machining with submicron range surface roughness. Analysis of mechanical properties and Weibull modulus of the green and sintered alumina samples after green state machining revealed that net shape forming via green machining of alumina using diamond embedded tool is viable.     

Synthesis of nanodiamond-reinforced aluminum metal matrix composites using cold-spray deposition

A dense nanodiamond–aluminum (ND–Al) composite coating was successfully produced by low pressure cold spray (CS) deposition of ball-milled powders containing 10 wt% ND. High-energy ball milling is a feasible means for the synthesis of composite feedstock powders as it provides excellent control over particle size distribution, crystal size, and the dispersion of ND agglomerates. The resulting CS coatings were characterized with respect to deposition efficiency, particle velocity and mechanical properties. It was found that the CS deposition produced dense, ND–Al composite coatings with increases in both hardness and elastic modulus as compared to the feedstock powders. The coating hardness of the 0.5 h-milled ND–Al composite that has the highest DE (14.2%) in ND–Al composites is 3.02 GPa, an 175% increase over the pristine as-received Al (1.10 GPa). The highest elastic modulus of the composite coatings is 98.3 GPa, a 51.5% increase over the as-received Al powder.     

Improvement of the adhesion of sputter-deposited cubic boron nitride films

Cubic boron nitride (cBN) thin films were grown on Si(100) and high-speed steel substrates by reactive r.f. sputtering in an Ar/N₂ discharge using an electrically conducting boron carbide (B₄C) target. The substrate electrode was grounded or operated either with a d.c. or an r.f. power supply. The deposition of cBN can be subdivided into three steps: (1) the growth of a thin, textured, hexagonal boron nitride (hBN) film, (2) the nucleation of cBN and (3) the growth of the cBN phase. As a measure of the cBN content, the ratio of the infrared absorption bands near 1100 cm⁻¹ (cBN) and 1400 cm⁻¹ (hBN) was used. The adhesion of cBN films is still an unsolved problem. Two aspects have to be considered: (1) the high intrinsic stress of the film and (2) the reactivity under humid conditions. We investigated the influence of the thickness, structure and surface roughness of hBN on the adhesion of cBN films. To modify the hBN films, the pressure, substrate bias and Ar/N₂ mixture was varied. Another way of improving the adhesion is plasma treatment of the cBN film directly after deposition. The process variations mentioned above increase the thickness of the adhering cBN films.     

Real indentation hardness of nano-polycrystalline cBN synthesized by direct conversion sintering under HPHT

The hardness characteristic of nano-polycrystalline cBN synthesized by direct conversion sintering was thoroughly investigated using Vickers and Knoop indenters. It was found that nano-polycrystals consisting of smaller cBN grains increase the elastic recovery of indentations during unloading of the indenters and the diagonal of Vickers indentations and the minor diagonal of Knoop indentations significantly decrease in length. Thus, if a Vickers indenter is used, the apparent hardness value increases, making it impossible to perform an accurate evaluation, e.g. incorrect Vickers hardness values in excess of 80 GPa were obtained from nano-polycrystalline cBN with a grain size of 50 nm or less. On the other hand, it was verified that a Knoop indenter ensures an accurate hardness evaluation even if the constituent grains are fine because its major diagonal length which is used for measurement is less susceptible to elastic recovery. In an accurate evaluation of the hardness of different types of nano-polycrystalline cBN using a Knoop indenter, the hardness of each type of cBN was around 45 GPa, and there was no clear Hall–Petch relationship between hardness and grain size without a slight bell-like correlation. These results suggest that reported hardness values higher than 80 GPa of similar nano-polycrystalline cBN evaluated using a Vickers indenter are incorrect values caused by elastic recovery occurring at the indentation.     

The effect of cellulose nanowhiskers on the flexural properties of self-reinforced polylactic acid composites

Self-reinforced polylactic acid (SR PLA) composites incorporating cellulose nanowhiskers (CNWs) were produced by coating orientated PLA fibres with a polyvinyl acetate (PVAc)–CNW mixture as a binder prior to hot compaction at 95 °C. PLA fibres were produced with an average diameter of 11 (±0.9) μm via a melt-drawing process at 180 °C. Scanning electron microscopy (SEM) images revealed that the CNWs imparted roughness to the PLA fibre surface. Cross-sectional examination of the SR PLA composites after hot-pressing confirmed that the PLA fibres had maintained their morphology. Incorporation of 8 wt% CNWs within the SR-PLA composites revealed an increase in their flexural strength (48%) and modulus (39%) compared to the control composite (flexural strength ∼82 MPa and modulus ∼3.9 GPa). In addition, whilst the control SR-PLA composite revealed quite brittle characteristics, the addition of CNWs and PVAc gave the self-reinforced composite a more ductile behaviour.