Wear mechanisms of TiN–TiB2 ceramic in sliding against alumina from room temperature to 700 °C

TiN–TiB₂ ceramic was prepared by the reactive hot-pressing method using titanium and BN powders as raw materials. The friction and wear properties of TiN–TiB₂ ceramic were evaluated in sliding against alumina ball from room temperature to 700 °C in air. The TiN–TiB₂ ceramic has a relative density of 98.6%, a flexural strength of 731.9 MPa and a fracture toughness of 8.5 MPa m^1/2 at room temperature. The TiN–TiB₂ ceramic exhibits a distinct decrease in friction coefficient at 700 °C as contrasted with the friction data obtained at room temperature and 400 °C. Wear mechanisms of TiN–TiB₂ ceramic depend mainly upon testing temperature at identical applied loads. Lubricious oxidized products caused by thermal oxidation provide excellent lubrication effects and greatly reduce the friction coefficient of TiN–TiB₂ ceramic at 700 °C. However, abrasive wear and tribo-oxidation are the dominant wear mechanisms of TiN–TiB₂ ceramic at 400 °C. Mechanical polishing effect and removal of micro-fractured grains play important roles during room-temperature wear tests.     

Spark plasma sintering of TiN–TiB2 composites

TiN–TiB₂ composites were fabricated by spark plasma sintering at 1773–2573 K. Effects of TiN and TiB₂ content on relative density, microstructure, and mechanical properties were investigated. Above 2373 K, TiN–TiB₂ composites exhibited relative densities over 95%. A high density of 99.7% was obtained at 2573 K with 20–30 vol% TiB₂. Shrinkage of the TiN–70 vol% TiB₂ composite was the highest at 1573–2473 K. For the TiN–70 vol% TiB₂ composite prepared at 1973–2373 K, TiN grains were small, while at 2573 K, TiB₂ became a continuous matrix, in which irregular-shaped TiN dispersed. hBN was formed in the TiN–TiB₂ composite containing 50–60 vol% TiB₂ above 2373 K. The maximum Vickers hardness and fracture toughness obtained for the TiN–80 vol% TiB₂ composite sintered at 2473 K was 26.3 GPa and 4.5 MPa m^1/2, respectively.     

Strengthening and toughening of TiN-based and TiB2-based ceramic tool materials with HfC additive

Effects of HfC addition on the microstructures and mechanical properties of TiN-based and TiB₂-based ceramic tool materials have been investigated. Their pore number decreased gradually and relative densities increased progressively when the HfC content increased from 15 wt% to 25 wt%. The achieved high relative densities to some extent derived from the high sintering pressure and the metal phases. HfC grains of about 1 µm evenly dispersed in these materials. Both TiN and TiB₂ grains become smaller with increasing HfC content from 15 wt% to 25 wt%, which indicated that HfC additive can inhibit TiN grain and TiB₂ grain growth, leading to the formation of a fine microstructure advantageous to improve flexural strength. Especially, TiB₂-HfC ceramics exhibited the typical core-rim structure that can enhance flexural strength and fracture toughness. The toughening mechanisms of TiB₂-HfC ceramics mainly included the pullout of HfC grain, crack deflection, crack bridging, transgranular fracture and the core-rim structure, while the toughening mechanisms of TiN-HfC ceramics mainly included pullout of HfC grain, fine grain, crack deflection and crack bridging. Besides, HfC hardness had an important influence on the hardness of these materials. Higher HfC content increased Vickers hardness of TiN-HfC composite, but lowered Vickers hardness of TiB₂-HfC composite, being HfC hardness higher than for TiN while HfC hardness is lower than for TiB₂. The decrease of fracture toughness of TiN-HfC ceramic tool materials with the increase of HfC content was attributed to the formation of a weaker interface strength.     

Spark plasma sintering of TiN ceramics codoped with SiC and CNT

In this research, we investigated the effects of SiC and multi-walled carbon nanotube (MWCNTs) addition on the densification and microstructure of titanium nitride (TiN) ceramics. Four samples including monolithic TiN, TiN-5?wt% MWCNTs, TiN-20?vol% SiC and TiN-20?vol% SiC-5?wt% MWCNTs were prepared by spark plasma sintering at 1900?°C for 7?min under 40?MPa pressure. X-ray powder diffraction patterns and scanning electron microscope (SEM) micrographs of the prepared ceramics showed that no new phase was formed during the sintering process. The highest calculated relative density was related to the TiN ceramic doped with 20?vol% SiC, while the sample doped with 5?wt% MWCNTs presented the lowest density. In addition, the SEM investigations revealed that the addition of sintering aids e.g. SiC and MWCNTs leads to a finer microstructure ceramic. These additives generally remain within the spaces among the TiN particles and prohibit extensive grain growth in the fabricated ceramics.     

Spark plasma sintering and mechanical properties of compounds in TiB2-SiC pseudo-diagram

The influence of spark plasma sintering (SPS) parameters (temperature, time, pressure) and the role of particle size on densification, microstructure and mechanical properties of commercial additive-free TiB₂, SiC and composites thereof were studied by X-ray diffraction, scanning electron microscopy, the ultrasonic method and indentation. Three particle sizes of SiC and 2 of TiB₂ were processed. An optimal cycle was found for TiB₂ and SiC: 2000?°C, 3?min dwell time, and 100?MPa applied at 600?°C. The relative density of pure SiC increases linearly from 70% to 90% when the initial particle size decreases from 1.75?µm to 0.5?µm. Pure TiB₂ was densified up to 87%. Using 2.5?wt% SiC in TiB₂, the relative density increases to 97%. Young's modulus and the hardness of all samples were measured, with results discussed. The higher properties were obtained for additive-free TiB₂–5%SiC with a relative density of 97% and with the Young's modulus and Vickers hardness values being close to 378?GPa and 23?GPa, respectively.     

Comparative investigation of microstructure,mechanical properties and strengthening mechanisms of Al-12Si/TiB2 fabricated by selective laser melting and hot pressing

Near-fully dense Al-12Si matrix composites reinforced with TiB₂ ceramic particles (2?wt%) were successfully fabricated by selective laser melting (SLM) and hot pressing (HP) of powder mixtures. TiB₂ ceramic particles are homogeneously distributed in the Al-12Si matrix at the micrometer-scale owing to a very good wetting between molten Al-12Si alloy and TiB₂ ceramic. The microstructural analysis of the as-fabricated SLM samples show the formation of a supersaturated α-Al phase and the decrease of free residual Si with respect to the hot-pressed ones. Both composites exhibit a fine microstructure with a grain size of ~?5.1?µm and ~?5.8?µm for SLM- and HP-fabricated samples with addition of TiB₂ ceramic particles. The SLM Al-12Si/TiB₂ composite exhibits significantly improved microhardness (~?142?±?6.0 HV_0.05) and yield strength (~247?±?4.0?MPa) compared to the corresponding HP one. Fine cell morphology and nanostructured dispersion strengthening are responsible for the improved mechanical strength of the Al-12Si/TiB₂ composite processed by SLM.     

Effect of PSO and TiB2 content on the high temperature adhesion strength of SiBCNO ceramic

In the present work, SiBCNO-based ceramic as high temperature adhesives are fabricated by polymer derived ceramic route. The effect of polysiloxane (PSO) and TiB₂ on the microstructure and high temperature strength is studied, and the toughing effect of TiB₂ is discussed. The highest adhesion strength of the joint (S12) reached up to 18.95?MPa at room temperature and 12.3?MPa at 1000?°C in vacuum after pyrolysis at 1000?°C in air for 2?h. It is interesting to find that the crystallization of nano-SiO₂ reinforces the strength and thermal stability of glass phase with the addition of PSO, besides, the TiB₂ plays the important role in improving adhesion strength by bearing load and facilitating the formation of stable SiO₂-B₂O₃-TiO₂ glass.     

Microstructural and mechanical characterization of spark plasma sintered TiC ceramics with TiN additive

This investigation intends to study the influence of titanium nitride (TiN) additive on the sintering behavior, mechanical features and microstructural development of TiC-based substances. For this objective, two different samples, namely monolithic TiC and TiC-5 wt% TiN, were sintered at 1900 °C using the SPS method. The specimens were held at the ultimate temperature for 10 min under 40 MPa. X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) were implemented to characterize the as-produced specimens. Introducing TiN increased the relative density of TiC by around 1.5%, standing next to 97%. The assessments revealed the creation of non-stoichiometric TiC_1-x along with some graphitized carbon phases in the undoped ceramic. By contrast, TiN additive completely dissolved into the TiC matrix in the composite sample and a new in-situ phase (C₃N₄) appeared. Finally, a Vickers hardness of ~2750 HV_0.1 and a flexural strength of ~450 MPa were achieved for the TiN-doped specimen.     

Densification improvement of spark plasma sintered TiB2-based composites with micron-, submicron- and nano-sized SiC particulates

Taguchi design of experiments methodology was used to determine the most influential spark plasma sintering (SPS) parameters on densification of TiB₂–SiC ceramic composites. In this case, four processing factors (SPS temperature, soaking time, applied external pressure and SiC particle size) at three levels were examined in order to acquire the optimum conditions. The statistical analysis identified the sintering temperature as the most effective factor influencing the relative density of TiB₂–SiC ceramics. A relative density of 99.5% was achieved at the optimal SPS conditions; i.e. temperature of 1800?°C, soaking time of 15?min and pressure of 30?MPa by adding 200-nm SiC particulates to the TiB₂ matrix. The experimental measurements and predicted values for the relative density of composite fabricated at the optimum SPS conditions and reinforced with the proper SiC particle size were almost similar. The mechanisms of sintering and densification of spark plasma sintered TiB₂–SiC composites were discussed in details.     

Enhanced densification of spark plasma sintered TiB2 ceramics with low content AlN additive

In the present study, we incorporated AlN (5 wt%) with TiB₂ ceramic and consolidated the mixture by relatively low temperature sintering method, resulting in a near fully dense composite. Monolithic TiB₂ and TiB₂–AlN (5 wt%) were manufactured by spark plasma sintering (SPS) at 1900 °C for 7 min under 40 MPa. The prepared composites were precisely characterized by field emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD) analyses. In addition, possible chemical reactions during the sintering process were thermodynamically assessed using the HSC Chemistry software. The addition of AlN influenced the sinterability of titanium diboride, yielding a relative density of 99.7%. XRD results revealed the in-situ formation of h-BN during the sintering, whereas thermodynamic studies suggested the formation of both Al₂O₃ and h-BN. Furthermore, the microstructural investigation verified the synthesis of both Al₂O₃ and h-BN phases. Finally, the fractographical study revealed the effective role of AlN additive for refining the microstructure of TiB₂.     

Microstructure and mechanical properties of spark plasma sintered TiB2 ceramics combined with a high-entropy alloy sintering aid

A high-entropy alloy (HEA), CoCrFeNiMn_0.5Ti_0.5, is used as a sintering aid for the densification of TiB₂ sintered by spark plasma sintering. The HEA content in the starting TiB₂-HEA mixture is varied from 0 to 10?wt-%. The microstructure and mechanical properties of the sintered samples are analysed and the optimum HEA content of 10% is found for the preparation of the TiB₂-HEA ceramics, allowing combining high mechanical properties (Vickers hardness of 2174.64?HV and flexural strength of 427.69?MPa) and high relative density of 99.1%.     

Selective laser melting of TiB2-Ti composite with high content of ceramic phase

An increasing need in customized ceramics and ceramic-metal composites has driven the development of powders feedstock and procedures for utilization of additive manufacturing for production of mechanically reliable composites. However, processing of materials with a high fraction of ceramic particles is still in its infancy. Herein we report on 3D printing of TiB₂-TiB-Ti composites from TiB₂-Ti powder mixture of high ceramic content (50 wt%TiB₂) by an optimized process of selective laser melting. In-situ synthesized from the mixture of commercially pure Ti and TiB₂ powders, the composites possess up to 20.4 GPa hardness despite of a relatively high porosity of around 8%. Improvement in hardness is mainly due to hardening effect of both TiB and TiB2 and correlated with an increase in fraction of needle-shaped TiB phase with an increase in laser energy density (LED). Depending on process parameters, an amount of the ceramic phases (needle-shaped TiB and coarse elongated TiB₂) can be customized. The laser energy density significantly affects the development of microstructure and size of the ceramic grains as well as the formation of solidification cracks. This study demonstrates the capacity of AM through SLM to produce the composites of high percentage of ceramic phase.     

Preparation and microstructure of 3D framework TiC–TiB2 ceramics and their reinforced steel matrix composites

An efficient method for in-situ fabrication of a three-dimensional framework based on heterogeneous TiC–TiB₂ materials with different B₄C content has been reported in the present study. Interpenetrating TiC–TiB₂/steel composites were subsequently prepared by infiltrating molten steel into TiC–TiB₂ framework. The XRD and SEM analyses confirmed that three-dimensional ceramics framework mainly consisted of heterogeneous TiC–TiB₂ phases with the ceramic particles closely connected with each other. TiC–TiB₂ ceramics framework exhibited a high porosity in the range 87.11%–95.95% and low bulk density of 0.17–0.22 g/cm³. The sample with ceramic framework containing 20 wt% B₄C exhibited the strongly continuous microstructure, whereas the sample with ceramic framework containing 25 wt% B₄C had the weakly continuous framework. The Vickers hardness and fracture toughness in the composites reached 284.5 HV and 23.7 MPa m^1/2, respectively. An optimal TiC: TiB₂ mass ratio of 37:55 could effectively inhibit the decomposition of TiB₂ in the molten steel. Inspecting the fracture surface, the dominated fracture modes was noted to be the quasi-cleavage and trans-granular dimple fracture, which could be attributed to novel three-dimensional bi-continuous structure formed between ceramic framework and steel substrate.     

High-strength TiB2-B4C composite ceramics sintered by spark plasma sintering

Spark plasma sintering (SPS) is an advanced sintering technique because of its fast sintering speed and short dwelling time. In this study, TiB₂, Y₂O₃, Al₂O₃, and different contents of B₄C were used as the raw materials to synthesize TiB₂-B₄C composites ceramics at 1850°C under a uniaxial loading of 48 MPa for 10 min via SPS in vacuum. The influence of different B₄C content on the microstructure and mechanical properties of TiB₂-B₄C composites ceramics are explored. The experimental results show that TiB₂-B₄C composite ceramic achieves relatively good comprehensive properties and exceptionally excellent flexural strength when the addition amount of B₄C reaches 10 wt.%. Its relative density, Vickers hardness, fracture toughness, and flexural strength reach to 99.20%, 24.65 ± .66 GPa, 3.16 MPa·m^1/2, 730.65 ± 74.11 MPa, respectively.     

Effects of additives on combustion synthesis of Al2O3–TiB2 ceramic composite

Al₂O₃, SiC and kaolin were employed as additives in combustion synthesizing Al₂O₃–TiB₂ ceramic composite. Effects of the additives on adiabatic temperature, combustion wave velocity, volume change and composite density were studied, and bending strength of the synthesized ceramics was evaluated. By theoretical calculation, the adiabatic temperature of Al–TiO₂–H₃BO₃ system is 2314.85 °C and decreases with increasing the additive addition. With Al₂O₃ addition, the phases presented in the ceramic composite are unchanged, and the phases of SiC and 3Al₂O₃·2SiO₂ emerges when SiC and kaolin are added. The addition of the additives results in a refined TiB₂ particulate size and reduces combustion wave velocity. The highest density is achieved with the addition of kaolin from 10 to 30 wt.% making the volume change from ?4.6 to ?1.2%. The bending strength of the TiB₂–Al₂O₃ composite is improved eight times with the addition of 30 wt.% kaolin.     

Interfacial microstructure and strengthening mechanism of BN-doped metal brazed Ti/SiO2-BN joints

Ag–Cu–Ti + BN composite filler was developed to braze SiO₂-BN ceramic and titanium. The effects of BN particles content on the microstructure and mechanical properties of the joints were investigated. The fine TiB whiskers and TiN particles were synthesized in the brazing seam by introducing BN particles. TiN–TiB₂ reaction layer formed adjacent to SiO₂-BN ceramic while Ti–Cu compound layer formed at Ti substrate. With the increase of BN content, more fine-grains formed in the joint and the reaction layer nearby the base materials became thinner. The hardness and modulus of the reaction phases were characterized by nanoindentations to reveal the plastic deformability of the brazing seam. The improvement of the joint strength was 340% with 3 wt.% BN addition. The joint strength was determined by the thermal expansion mismatch between the joined materials, plastic deformation in the brazing seam, and interfacial structure of the joint.     

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 TiB2 content on microstructure and hardness of TiB2-B4C composite

In this study a composite ceramic powder mixture using fine powders of titanium diboride (TiB₂) and boron carbide (B₄C) was consolidated to theoretical density using the technique of plasma pressure compaction. Achieving rapid consolidation of the composite powder mixture is an essential requirement for achieving microstructural control and better mechanical properties in the consolidated end product. The variables chosen in making the composite samples was the titanium diboride (TiB₂) content. The microstructure and hardness of the ceramic composite sample made by consolidating various powder mixtures at a temperature of 1700 °C are compared. Microhardness measurements reveal a gradual increase in hardness with an increase in TiB₂ content in the starting powder mixture. The specific role of TiB₂ content in influencing microstructural development and hardness is presented and discussed.     

Microstructure and mechanical properties of B4C–TiB2 ceramic composites prepared via a two-step method

B₄C–TiB₂ ceramic composites were fabricated by a two-step method. First, B₄C–TiB₂ composite powders were synthesized from TiC–B powder mixtures at 1400 ℃, then mixed with commercial B₄C powders by ball milling and the B₄C–TiB₂ ceramic composites were prepared by hot pressing at 1950 ℃. This two-step method not only effectively refined TiB₂ grains, but also allowed the composition of the composites to be freely designed. The microstructure and mechanical properties of the composites were investigated. The results showed that the B₄C–TiB₂ ceramic composite with a 10 wt% TiB₂ content obtained the ideal comprehensive performance, with a volume density, Vickers hardness, bending strength, and fracture toughness of 2.61 g/cm³, 35.3 GPa, 708 MPa, and 5.82 MPa m^1/2, respectively. The advantages of the in-situ reaction process were fully exerted by the two-step method, which made a remarkable contribution to the excellent properties of B₄C–TiB₂ ceramic composites.     

Microstructures and mechanical properties of B4C–SiC and B4C–SiC–TiB2 ceramic composites fabricated by hot pressing

Boron carbide (B₄C) ceramic composites with excellent mechanical properties were fabricated by hot-pressing using B₄C, silicon carbide (SiC), titanium boride (TiB₂), and magnesium aluminum silicate (MAS) as raw materials. The influences of SiC and TiB₂ content on the microstructural evolution and mechanical properties of the composites were systematically investigated. The mechanism by which MAS promotes the sintering process of composites was also investigated. MAS exists in composites in the form of amorphous phase. It can effectively remove the oxide layer from the surface of ceramic particles during the high temperature sintering process. The typical values of relative density, hardness, bending strength, and fracture toughness of B₄C–SiC–TiB₂ composites are 99.6%, 32.61 GPa, 434 MPa, and 6.20 MPa m^1/2, respectively. Based on the microstructure observations and finite element modeling, the operative toughening mechanism is mainly attributed to the crack deflection along the grain boundary, which results from the residual stress field generated by the thermal expansion mismatch between B₄C and TiB₂ phase.