Documentation of tool wear progress in the machining of nodular ductile iron with silicon nitride-based ceramic tools

Nowadays, the HPM of cast irons is based on silicon nitride ceramic and CBN cutting tools. This paper characterizes and correlates several outputs of the cutting process of nodular cast iron using uncoated and Al₂O₃/TiN coated Si₃N₄ ceramic tools resulting from wear progress and destruction of tool faces. Investigations include tool wear curves, tribological behaviour of the tool–chip interface and tool wear mechanisms occurring on contact surfaces. The image-based characterization of worn surfaces employs such techniques as SEM, BSE and EDX analysis. The occurrence of various wear mechanisms, such as abrasive, adhesive and chemical wear was revealed.     

Machining performance of pearlitic–ferritic nodular cast iron with coated carbide and silicon nitride ceramic tools

This paper concerns the fundamental cutting characteristics obtained in the turning of the pearlitic–ferritic nodular iron (EN-GJS-500-7 grade with UTS=500 MPa) when using carbide tools coated with single TiAlN and multilayer TiC/Ti(C,N)/Al₂O₃/TiN coatings, as well as silicon nitride (Si₃N₄) based ceramic tools. As a competitor, a P20 uncoated carbide grade was selected. The fundamental process readings include cutting and feed forces, the tool–chip interface temperature, Peclet number, friction coefficient and the tool–chip contact length as functions of cutting parameters. In particular, the measurements of cutting temperature were carried out using conventional tool–work thermocouple method and IR thermography. It is concluded based on many process characteristics that multilayer coated and ceramic tools can substantially improve the performance of nodular iron machining.     

Mechanical property and cutting performance of yttrium-reinforced Al2O3/Ti(C,N) composite ceramic tool material

Effects of yttrium on the mechanical property and the cutting performance of Al₂O₃/Ti(C,N) composite ceramic tool material have been studied in detail. Results show that the addition of yttrium of a certain amount can noticeably improve the mechanical property of Al₂O₃/Ti(C,N) ceramic material. As a result, the flexural strength and the fracture toughness amount to 1010 MPa and 6.1 MPam^1/2, respectively. Cutting experiments indicate that the developed ceramic tool material not only has better wear resistance but also has higher fracture resistance when machining hardened #45 steel. The fracture resistance of the yttrium-reinforced Al₂O₃/Ti(C,N) ceramic tool material is about 20% higher than that of the corresponding ceramic tool material without any yttrium additives.     

Reticulated Porous Multiphase Ceramics with Improved Compressive Strength and Fracture Toughness

A multiphase reticulated porous ceramic (RPC) as Si₃N₄–Al₂O₃–SiO₂ was fabricated by replication techniques. Proper volumes of additives and twice sinter- twice immerse process endow the RPC an excellent crack healing and submerging property. The compressive strength and fracture toughness improved owing to the crack bridging behavior. The existence of pores in struts in RPC blunt the crack tip and increased the external force needed to propagate the crack. The mechanisms play a beneficial role in enhancing the compressive strength and fracture strength. Si₃N₄ RPC with additives of 5%Al and 5% Al₂O₃ yielded the compressive strength of 9.8 MPa and fracture toughness of 0.3 MPa m^1/2.     

High α-β phase transition and properties of YbF3-added porous Si3N4 ceramics obtained by low temperature pressureless sintering

In this paper, we used YbF₃ as a sintering additive to get a high α-β phase transition in porous Si₃N₄ ceramics. The mechanism of YbF₃ as sintering additives as well as the relationship between microstructure and mechanical properties have been investigated in detail. In addition, we used pressureless sintering to lower the temperature to 1550 °C. YbF₃ makes α-Si₃N₄ completely transform to β-Si₃N₄, whereas only 41.1% β-Si₃N₄ could be obtained with Yb₂O₃. This process yielded ceramics with more flexural strength and increased fracture toughness using less energy. In addition, using YbF₃ substituted for part Yb₂O₃ could promote sintering behaviors of Si₃N₄ ceramics at low temperature to increase α-β phase transition rate and improve the properties of silicon nitride ceramics significantly. In particular, when we used YbF₃-Yb₂O₃ as additives, we obtained a flexural strength of 269.87 MPa and a fracture toughness of 4.59 MPa·m^1/2.     

Mechanical properties improvement related to the isothermal holding time in Si3N4 ceramics sintered with an alternative additive

In the present work, the influence of the isothermal holding time on the physical (relative density and mass loss), chemical (α–β transformation and intergranular phase crystallization) and mechanical (hardness and fracture toughness) properties of Si₃N₄ ceramics with Al₂O₃ and CTR₂O₃ as additives has been studied. CTR₂O₃ is a natural rare earth oxide mixture, produced at DEMAR-FAENQUIL from the mineral xenotime, consisting mainly of Y₂O₃, Yb₂O₃, Er₂O₃ and Dy₂O₃. The increase in hardness and fracture toughness with increasing duration of isothermal sintering is discussed in regard of densification, α–β Si₃N₄ phase transformation and microstructure. The microstructural variations were decisive for the increase of fracture toughness, because larger grains (>4 μm) with higher aspect ratios (>6) developed during increased sinter periods, enhancing crack deflection and crack-bridging mechanism. In this way longer isothermal holding times contribute to the improvement of the physical and mechanical properties of silicon nitride based ceramics.     

Thermal shock behavior of Si3N4-TiN nano-composites

Si₃N₄-TiN nano-composites were fabricated by hot press sintering nano-sized Si₃N₄ and TiN powders. The microstructure, mechanical properties and thermal shock behavior of Si₃N₄-TiN nano-composites were investigated. The addition of proper amount TiN particles can significantly increase the flexural strength and the fracture toughness. Si₃N₄-TiN nano-composites showed both higher critical temperature difference and higher residual strength compared with those of monolithic silicon nitride nano-ceramic when the amount of TiN is less than 15 wt.%. But a further increase in the amount of TiN leaded to a decrease in the thermal shock resistance.     

Oxidation and corrosion of silicon nitride ceramics with different sintering additives at 1200 and 1500 °C in air, water vapour, SO2 and HCl environments - A comparative study

The effect of different sintering additives on the high temperature oxidation and corrosion behaviour of silicon nitride based ceramics was investigated. Comparative tests were conducted at 1200 and 1500 °C in air, in water vapour, and with the highly corrosive gases HCl and SO₂. Si₃N₄ was prepared with MgO, Al₂O₃, Y₂O₃ and Al₂O₃ + Y₂O₃ sintering additives. Hot pressed discs were tested for a total time of up to 128 h. The electrically conductive ceramic composites Si₃N₄ + TiN and Si₃N₄ + MoSi₂ were also tested under the same conditions. The effects that the different corrosion environments have on the different ceramics are presented. SEM studies of the oxidised ceramics show the direct transformation of Si₃N₄ grains into SiO₂ through a reaction interface layer.     

Effects of sintering aides on the hydrothermal oxidation of silicon nitride spherical rolling elements

Commercially available silicon nitride (Si₃N₄) spherical bearing rolling elements containing TiO₂, Y₂O_3, MgO and Al₂O₃ additives were evaluated for corrosion-resistance in high-temperature, high-pressure hydrothermal tests designed to simulate aero propulsion conditions. Spheres were exposed in an autoclave at 523–623?K and 5.2–16.5?MPa for 12–48?h and characterised using mass change and pH measurements, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy and inductively coupled plasma mass spectrometry. The oxidation resistance of the TiO₂/Y₂O₃/Al₂O₃-sinter-aided Si₃N₄ ceramic closely matches the Y₂O₃/Al₂O₃-doped Si₃N₄ and outperforms the MgO-sinter-aided Si₃N₄. Additional studies on the TiO₂/Y₂O₃/Al₂O₃ Si₃N₄ composition show pitting initiates around titanium-rich inclusions, due to a break in the protective hydroxide layer, accessible diffusion paths around inclusions and the catalytic nature of titanium. This study demonstrates that the addition of TiO₂/Y₂O₃/Al₂O₃ to hot pressed Si₃N₄ reduces corrosion rates in high-temperature, high-pressure, hydrothermal environments.     

Mechanical properties and microstructure of Al2O3/Ti(C,N)/CaF2@Al2O3 self-lubricating ceramic tool

Due to the poor mechanical properties of solid lubricants, direct addition to the ceramic matrix will reduce the mechanical properties of the material. In this study, Al(OH)₃ was coated on the surface of nano CaF₂ by non-uniform nucleation method and added to Al₂O₃/Ti(C,N) ceramic matrix. Al₂O₃/Ti(C,N)/CaF₂@Al₂O₃ was prepared by vacuum hot pressing sintering. Compared with the material directly added with nano-solid lubricant, the mechanical properties of ceramic tools added with coated nano-solid lubricant have been significantly improved. Among them, when the content of coated nano-solid lubricant is 10 vol%, the ceramic material has better comprehensive mechanical properties. SEM observation shows that the cross-sectional particle distribution of nano-coated powder ceramic material is relatively uniform and has good compactness. The fracture mode of ceramic materials is a mixed fracture mode of intergranular fracture and transgranular fracture.     

The influence of powder characteristics on mechanical properties of Al2O3–TiC–Co ceramic materials prepared by Co‐coated Al2O3/TiC powders

Ultrafine Al₂O₃–TiC–Co (ATC) ceramic is prepared in order to improve the bending strength and fracture toughness of ceramic materials. The ultrafine Co‐coated Al₂O₃ and TiC powders have been synthesized by electroless plating at room temperature, and the composite powders were sintered by hot‐pressing to compact ATC samples. The average bending strength, average hardness and average fracture toughness values of ATC ceramic with different particle sizes and Co contents were investigated. The toughening mechanism of the ultrafine ATC ceramic was studied by transmission electron microscopy (TEM) and ceramic performance testing methods. The results show that the relative density, bending strength and fracture toughness values increase remarkably with the increase of Co content. The ultrafine grain of original powders is beneficial to improve the relative density, strength and toughness values of ATC ceramic. The Co phase hinders the growth of ATC ceramic grains during sintering. The Co phase forms a three‐dimensional mesh skeleton structure during sintering, improving the fracture toughness and strength of the composite ceramic.     

Gradients in elastic modulus for improved contact-damage resistance. Part I: The silicon nitride–oxynitride glass system

Silicon nitride (Si₃N₄)-based graded materials were fabricated with controlled, unidirectional gradients in elastic modulus from the surface to the interior. This was accomplished by infiltrating a low modulus silicon oxynitride glass into a dense, higher modulus, Si₃N₄ ceramic. Elastic Hertzian indentation (spherical indenter) experiments were performed on both the graded and the monolithic Si₃N₄. While Hertzian indentation of the monolithic ceramic resulted in classical cone cracks, such cracks were completely suppressed in the graded materials at comparable load levels, despite the lower strength and lower toughness of the surface layer comprising glass. Finite element analysis (FEA) of the stresses associated with the indentation was also performed to gain insight into the mechanism for the enhanced contact damage resistance in the graded materials. The computational analysis revealed that the maximum tensile stresses outside the Hertzian contact circle, which drive the cone-cracks, are reduced by approximately 30% relative to those present in the monolithic silicon nitride. This reduction in the tensile stresses more than compensates for the lower toughness at the graded material surfaces, relative to the monolithic Si₃N₄. The FEA also allowed us to develop some strategies for elastic–modulus-gradients that would lead to further improvements in the cone-crack suppression characteristics of graded materials in general.     

Mechanical behavior of 3Al2O3·2SiO2 films under nanoindentation

A complete and systematic nanoindentation study was conducted on a mullite (3Al₂O₃·2SiO₂) coating ～1 μm thick, deposited by means of chemical vapor deposition on a silicon carbide (SiC) substrate. The investigation included using different indenter tip geometries (Berkovich, spherical and cube-corner), complemented with atomic force microscopy and three-dimensional focused ion beam tomography to characterize the indentation response, deformation and damage micromechanisms. The intrinsic mechanical properties of the 3Al₂O₃·2SiO₂ film and the interfacial toughness of the coated (3Al₂O₃·2SiO₂/SiC) system were critically evaluated to assess the influence of substrate and film residual stresses. Through appropriate implementation of specific indenter tip geometry, different length-scale mechanical properties in the materials studied were successfully determined: yield strength and fracture toughness for the film, together with energy of adhesion per unit area and interface fracture toughness for the coated system.     

Effect of Al2O3 addition on properties of non-sintered SiC–Si3N4 composite refractory materials

Preparation of SiC–Si₃N₄ composite refractory materials without sintering entails only low energy consumption and incurs little cost compared with traditional preparation methods. This paper investigated the effect of Al₂O₃ addition on bulk density, apparent porosity, linear shrinkage and oxidation resistance of as-fabricated non-sintered SiC–Si₃N₄ composite refractory materials. Meanwhile, the compressive and flexural strengths both before and after heat treatment were analyzed. The mechanisms of oxidation resistance and cryolite resistance of the SiC–Si₃N₄ composite refractory materials are discussed. Increasing amounts of Al₂O₃ reduced linear shrinkage but increased oxidation resistance and cryolite resistance. Moreover, compressive and flexural strengths initially increased and then decreased, with maximum values achieved at an Al₂O₃ addition of 8% w/w.     

Densification, microstructure, and fracture behavior of TiC/Si3N4 composites by spark plasma sintering

TiC/Si₃N₄ composites were prepared using the β-Si₃N₄ powder synthesized by self-propagating high-temperature synthesis (SHS) and 35 wt.% TiC by spark plasma sintering. Y₂O₃ and Al₂O₃ were added as sintering additives. The almost full sintered density and the highest fracture toughness (8.48 MPa·m^½) values of Si₃N₄-based ceramics could be achieved at 1550°C. No interfacial interactions were noticeable between TiC and Si₃N₄. The toughening mechanisms in TiC/Si₃N₄ composites were attributed to crack deflection, microcrack toughening, and crack impedance by the periodic compressive stress in the Si₃N₄ matrix. However, increasing microcracks easily led to excessive connection of microcracks, which would not be beneficial to the strength.     

Effect of sintering temperature on the structure and properties of polycrystalline cubic boron nitride prepared by SPS

The polycrystalline cubic boron nitride (PcBN) with Si₃N₄–AlN–Al₂O₃–Y₂O₃ ceramic system as binding agents was prepared by spark plasma sintering (SPS). The starting materials Si₃N₄, AlN, Al₂O₃, Y₂O₃, and cBN in the ratio of 22:14:10:4:50 were heated to a sintering temperature between 1250 °C and 1450 °C at a heating rate of 300 °C/min, with a holding time of 5 min in nitrogen atmosphere. The microstructure, phase constitution, microhardness and fracture toughness of the prepared PcBN were then studied. It was shown that the Si₃N₄–AlN–Al₂O₃–Y₂O₃–cBN polycrystalline materials were densified in a very short sintering time resulting in materials with relative densities of more than 95%. When the sintering temperature increased, the microhardness and fracture toughness of prepared PcBN were also increased. The microhardness of PcBN prepared at 1250–1450 °C was between 28.0 ± 0.5 GPa and 48.0 ± 0.9 GPa, and its fracture toughness K_IC was from 7.5 ± 0.2 MPa m^1/2 to 11.5 ± 0.3 MPa m^1/2. Microstructure study showed that the ceramic-binding agents bonded with cubic boron nitride particles firmly. Our work demonstrated that spark plasma sintering technology could become a novel method for the preparation of PcBN cutting materials.     

The influence of the grain boundary phase on the mechanical properties of Si3N4–MoSi2 composites

The microstructure and mechanical properties of Si₃N₄–MoSi₂ composites doped with two different sintering additive systems, Y₂O₃–Al₂O₃ and Lu₂O₃, were investigated. It was found that the composite doped with Y₂O₃–Al₂O₃ had an amorphous grain boundary phase, while the grain boundary phase of the Lu₂O₃-doped composites was completely crystallized. The Si₃N₄–MoSi₂ composite containing Lu₂O₃ had higher elastic modulus and better creep resistance at elevated temperatures (>1000 °C) than the composite doped with Y₂O₃–Al₂O₃. This is attributed to the crystallization and higher softening temperature of the Lu₂O₃-doped grain boundary phase compared with that doped with Y₂O₃–Al₂O₃. However, the toughness and strength were not influenced significantly by the grain boundary phase. The inclusion of MoSi₂ particles in Si₃N₄ can improve their fracture toughness through residual stresses induced by the coefficient of thermal expansion mismatch of Si₃N₄ and MoSi₂. The strength decreased significantly at temperatures over 1000 °C due to the brittle–ductile transition of the MoSi₂ phase.     

Fabrication and properties of Si3N4 based ceramics using combustion synthesized powders

Silicon nitride (Si₃N₄) based ceramics were fabricated with β-SiAlON and Si₃N₄ powders synthesized by combustion synthesis method via power injection molding (PIM). In the PIM process, the solids loading for each material was first determined from the results of the torque rheometer experiment. The mixing process was repeated to produce the homogeneous feedstock, and homogeneity of feedstocks was evaluated by observing the shear viscosity with time at a constant shear rate. The rheological behavior of feedstocks was investigated using capillary rheometer. It found that both feedstocks have no problem in injection molding. The binder decomposition behavior was also investigated, and a wax-polymer binder system was nearly removed by the optimized solvent and thermal debinding processes. Thereafter, the debound samples were sintered at 1750 and 1800 °C for 4 h in nitrogen atmosphere. Regardless of sintering temperature, the relative density of higher than about 96% was achieved. When comparing mechanical properties including bending strength, Vickers hardness and fracture toughness, Si₃N₄ with 2 wt% Y₂O₃ and 5 wt% Al₂O₃ (Si₃N₄+2Y5A) had higher values than β-SiAlON with 4 wt% Y₂O₃ (β-SiAlON+4Y) regardless of sintering temperature. It was supported by observing the microstructures of the plasma-etched samples.     

Development of Si3Na/Al composite by pressureless melt infiltration

Pressureless infiltration process to synthesize Si3N4/Al composite was investigated. Al-2%Mg alloy was infiltrated into Si3N4 and Si3N4 containing 10% Al2O3 preforms in the atmosphere of nitrogen. It is possible to infiltrate Al-2%Mg alloy in Si3N4 and Si3N4 containing 10% Al2O3 preforms. The growth of the dense composite of useful thickness was facilitated by the presence of magnesium powder at the interface and by flowing nitrogen. During infiltration Si3N4 reacted with aluminium to form Si and AIN, the growth of composite was found to proceed in two ways, depending on the Al2O3 content in the initial preform. Firstly, preform without Al2O3 content gives rise to AIN, Al3.27Si0.47 and Al type phases after infiltration. Secondly, perform with 10% Al2O3 content gives rise to AIN-Al2O3 solid solution phase （AION）, MgAl2O4, Al and Si type phases. AlON phase was only present in composite, containing 10% Al2O3 in the Si3N4 preforms before infiltration.     

Thermal plasma synthesis of SiC- Si3N4 composite powders from SiCH3CI3- NH3- H2

SiC-Si₃N₄ composite powders were synthesized by introducing trichloromethylsilane, ammonia, and hydrogen into a high-temperature radiofrequency (RF) thermal plasma argon gas. Powders were characterized by XRD, TEM, and FT-IR. Silicon carbide and silicon nitride were formed independently into separate powders. Silicon carbide was formed as β-SiC crystalline powder and silicon nitride was in an amorphous state. The crystalline SiC powders were in the size range of 75 to 200 nm and amorphous Si₃N₄ powders were 5 to 60 nm. When the mole ratio of ammonia to trichloromethylsilane was between 1 and 2, SiC-Si₃N₄ composite powders were formed, and when it was higher than 4, Si₃N₄ powders were formed.