Structural correlations at Si/Si3N4 interface and atomic stresses in Si/Si3N4 nanopixel-10 million-atom molecular dynamics simulation on parallel computers

We have combined first-principle calculations of charge transfer at the Si/Si₃N₄ interface with the interaction potential models for bulk Si and Si₃N₄ to produce a model for the Si/Si₃N₄ interface. Using these interatomic potentials, million atom molecular dynamics simulations have been performed to characterize the structure of Si(111)/Si₃N₄(0001) and the Si(111)/a-Si₃N₄ interfaces. Ten million-atom simulations are performed using multiresolution molecular-dynamics method on parallel computers. Atomic stress distributions are determined in a 54 nm nanopixel on a 0·1 μm silicon substrate. Effects of surfaces, edges, and lattice mismatch at the Si(111)/Si₃N₄(0001) interface on the stress distributions are also investigated. Stresses are found to be highly inhomogeneous in the nanopixel—the top surface of silicon nitride has a compressive stress of +3 GPa and the stress is tensile, −1 GPa, in silicon below the inter-face. These simulation methods can also be applied to other semiconductor/ceramic interfaces as well as to metal/ceramic and ceramic/ceramic interfaces.     

Probing the Conductance and Microstructure Heterogeneity of Si3N4/TiC‐Based Nanocomposite at the Nanoscale by Scanning Impedance Microscopy

This study presents the results of atomic force microscopy (AFM)‐localized impedance measurements within Si₃N₄/glassy phase/TiC heterogeneous nanostructures. The three phases show significant differences in the charge‐transfer resistance and interface capacitance values detected on the plasma‐etching surface by an ultrasharp AFM, and these characteristics are helpful to understand the sintering behavior in spark plasma sintering. The effect of an electrical field may induce localized Joule heating on conductive nano‐TiC embedded in the Si₃N₄‐based matrix. The glassy phase doped with Ti and C, as observed by transmission electron microscopy, may promote electrowetting, leading to enhanced densification in the insulating/conductive ceramic nanocomposite system.     

Fabrication of Si3N4–SiBC composite ceramic and its excellent electromagnetic properties

To obtain better electromagnetic wave absorbing property, it is vitally necessary to develop novel ceramics with not only high dielectric loss but also low dielectric constant. Si₃N₄–SiBC, a composite ceramic with such dielectric properties, was fabricated by infiltrating SiBC into porous Si₃N₄ ceramic via low pressure chemical vapor infiltration. The high dielectric loss and the low dielectric constant are attributed to the unique microstructure of SiBC, which also leads to a very excellent wave-absorbing property of Si₃N₄–SiBC ceramic, attaining a minimal reflection coefficient of ?28 dB. Besides, the Si₃N₄–SiBC ceramic also shows a high mechanical property. Therefore, the Si₃N₄–SiBC ceramic exhibits great potential as an excellent functional and structural ceramic.     

Laser-induced metallization of porous Si3N4 ceramic and its brazing to TiAl alloy

The poor wettability of traditional brazing filler alloys on the surface of ceramics always lead to the formation of defects in the joints and weaken the bonding strength eventually, especially the porous ceramics. Metallization on ceramics is an effective way to improve the wettability. In this work, laser-induced cladding process was applied to metalize the surface of porous Si₃N₄ ceramic, and the traditional AgCu eutectic filler alloy can wet on the metalized surface completely. The metalized porous Si₃N₄ ceramic brazed to TiAl alloy successfully using AgCu filler alloy. The interfacial microstructure and mechanical property of the porous Si₃N₄/TiAl alloy brazed joint was significantly improved by the novel laser-induced metallization process.     

Experimental determination of residual stress in silicon nitride diffusion bonds obtained by high-energy X-ray diffraction

High resolution X-ray scanning diffractometry has been used to study the residual strain in binary metal/ceramic (Ni/Si₃N₄) and ceramic/ceramic (Si₃N₄/Ni thin film/Si₃N₄) diffusion bonds. Bonds were fabricated by simultaneous high temperature heating and uniaxial pressing. The axial and radial strain profiles have been determined along selected lines perpendicular to the bonding interface inside the ceramic bodies. The X-ray experiments have been done at the energy of 60 keV, which assured a very small absorption, and therefore, strain fields have been measured in the ceramic bulk. Strains showed higher values near the interface that decreased with the distance.     

Cutting performance and tool wear of SiAlON and TiC-whisker-reinforced Si3N4 ceramic tools in side milling Inconel 718

Cutting performance and tool wear of two ceramic tools, SiAlON and TiC-whisker-reinforced Si₃N₄, in the side milling processes of Inconel 718 are evaluated in comparison, including cutting force, temperature, surface morphology, tool wear and corresponding mechanism. Results show that these two ceramic tools has advantages and disadvantages respectively, due to the properties of ceramic matrixes and the evolutions of build-up edges. SiAlON ceramic tool has better resistance to wear, but causes poor surface quality. TiC-whisker-reinforced Si₃N₄ ceramic tool generates better surface quality, but bears severe wear. Brittle damage, as the main mode of wear, occurs to both ceramic tools in different formations. SiAlON ceramic tool is featured by crater-like damage on blades while TiC-whisker-reinforced Si₃N₄ ceramic tool is featured by whole-layer damage on flank faces.     

Phase transformation and interface segregation behavior in Si3N4 ceramics sintered with La2O3–Lu2O3 mixed additive

Microstructure and mechanical property of silicon nitride (Si₃N₄) ceramic are strongly dependent on the selection of sintering additives. When rare‐earth (RE) oxide is used as the sintering additive, segregation of RE ions at interface between Si₃N₄ grain and intergranular glassy film (IGF) is believed to play a critical role. Although the ionic radius of RE ion is known to be an empirical parameter to modify the mechanical property, the correlation between the segregated ions and their ionic radii is still under controversy. In order to address this issue, (i) rate of α‐β phase transformation and (ii) segregation behavior at the interface were studied for Si₃N₄ ceramics sintered using mixture of La₂O₃ and Lu₂O₃ as additives in this study. Specimens of Lu content 30% and higher exhibited lower activation energies for the α‐β phase transformation as compared with those of Lu content 20% and lower. In terms of the segregation behavior, La was preferably segregated at one site and Lu at the other site along β‐Si₃N₄/IGF interface in the specimens of Lu content 30% and higher. It is understood from these results that Lu segregation site should be more closely related with grain growth.     

Stereolithographical fabrication of dense Si3N4 ceramics by slurry optimization and pressure sintering

Photocurable gray-colored Si₃N₄ ceramic slurry with high solid loading, suitable viscosity and high curing depth is critical to fabricate dense ceramic parts with complex shape and high surface precision by stereolithography technology. In the present study, Si₃N₄ ceramic slurry with suitable viscosity, high solid loading (45 vol %) and curing depth of 50 μm was prepared successfully when surface modifier KH560 (1 wt%) and dispersant Darvan (1 wt%) were used. The slurry exhibits the shear thinning behavior. Based on the Beer-Lambert formula, D_p (the attenuation length) and E_c (the critical energy dose) of Si₃N₄ ceramic slurry with solid loading of 45 vol % were derived as 0.032 mm and 0.177 mJ/mm², respectively. Si₃N₄ ceramic green parts with complex shape and high surface precision were successfully fabricated by stereolithography technology. After optimizing the debinding and sintering process for green parts, dense Si₃N₄ ceramics with 3.28 g/cm³ sintering density were fabricated. The microhardness and fracture toughness of as-sintered Si₃N₄ ceramics are ~14.63 GPa and ~5.82 MPa m^1/2, respectively, which are comparable to those of the samples by traditional dry-pressed and pressureless sintering technology. These results show that ceramic stereolithography technology could be promising to fabricate high performance ceramics, especially for gray-colored monolithic Si₃N₄ ceramics.     

Additive manufacturing of silicon nitride ceramics: A review of advances and perspectives

Silicon nitride (Si₃N₄) ceramic has been widely applied in various engineering fields. The emergence of additive manufacturing (AM) technologies provides an innovative approach for the fabrication of complex-shaped Si₃N₄ ceramic components. This article systematically reviews the advances of the AM of Si₃N₄ ceramic in recent years and forecasts the potential perspectives in this field. This review aims to motivate future research and development for the AM of Si₃N₄ ceramic.     

Toughening of silicon nitride ceramics by addition of multilayer graphene

Silicon nitride (Si₃N₄) ceramics have superior mechanical properties allowing their broad application in many technical fields. In this work, Si₃N₄-based composites with 1–5?wt% multilayer graphene (MLG) content were fabricated by spark plasma sintering at different temperatures and holding time in order to improve the fracture resistance of the Si₃N₄ ceramic. Our investigation focused on understanding the relationships between the microstructure and mechanical properties with special attention to the intergranular phases between Si₃N₄ matrix and MLG reinforcement.We have found that nanopores developed at the Si₃N₄-MLG interface due to a reaction between carbon and the oxygen available in the topmost layer of the Si₃N₄ particles. Interface porosity has an optimum for the toughening effect. In 1?wt% MLG/Si₃N₄ composites nanopores are local, but separated at the Si₃N₄-MLG interface, which promote the MLG pull-out mechanism imparting a significant toughening effect on the composite. Beyond the optimal 1?wt% MLG content, MLG platelets agglomerate and excessive porosity are developed at the Si₃N₄-MLG interfaces, leading to weaker matrix- graphene adhesion and thus lower fracture toughness.     

Improving cure performance of Si3N4 suspension with a high refractive index resin for stereolithography-based additive manufacturing

Silicon nitride (Si₃N₄) slurries with high solid loading, low viscosity and good stability is difficulty prepared, due to low intrinsic surface charge and a large refractive index (RI) difference between Si₃N₄ powder and resin. In this paper, the curing behavior of Si₃N₄ slurry with different functional group and RI of resin monomer were systematically researched, and then the kind and optimum content of dispersant were investigated. Subsequently, a high solid loading Si₃N₄ slurry (44 vol%) with good curing behavior, low viscosity and favorable stability was successfully prepared. Lastly, the dense Si₃N₄ ceramic parts were fabricated by the suitable Si₃N₄ slurry (44 vol%) via stereolithography. After debinding and sintering process, the relative density and flexural strength of Si₃N₄ ceramic were 98.28% and 800 ± 27.28 Mpa, respectively.     

Friction and wear properties of Si3N4-hBN ceramic composites using different synthetic lubricants

This paper presents a tribological investigation of Si₃N₄-hBN composite ceramics using synthetic lubricants. The friction and wear properties of Si₃N₄-hBN ceramic composites sliding against TC4 titanium alloy (Ti6Al4V) were investigated via pin-on-disc tests. An axial compressive load of 10?N was applied with a sliding speed of 0.73?m/s. Three different lubrication conditions including simulated body fluid (SBF), physiological saline (PS) and bovine serum (BS) were used. For SBF lubrication, the friction coefficients and wear rates of Si₃N₄-hBN/Ti6Al4V pairs were varying with the increase of hBN contents. When using 20?vol% hBN, the average friction coefficient and wear rate of Si₃N₄ (0.28 and 3.5?× 10^?4 mm³ N^?1 m^?1) were as good as that of the pure Si₃N₄ (0.34 and 3.69?× 10^?4 mm³ N^?1 m^?1). Meanwhile, the processability of the Si₃N₄ material would be improved by adding hBN. It was worth to mention that when using 30?vol% hBN, the tribological performance of bearing combination deteriorated with extensive wear from the ceramic pin. This may due to the reduction of mechanical property caused by adding hBN and the occurring of tribochemical reaction. According to the worn surface examination and characterization, the main wear mechanism was abrasive and adhesion wear. Scratch grooves were observed on the metal disc, and metallic transform layers were seen on the ceramic pin. Moreover, surface lubrication film consisting of TiO₂, SiO₂·nH₂O, Mg(OH)₂, and H₃BO₃ were formed on the metal disc when using SBF lubrication and 20?vol% hBN content. Among the three lubrication conditions, SBF generally led to the best tribological performance. No surface lubrication film was found during BS and PS lubrications. This may be resulted from the absence of essential ions to promote the formation of surface lubrication film (PS lubrication) and the formation of a protein barrier on the surface of the metal disc (BS lubrication).     

Ultralight Silicon Nitride Ceramic Foams from Foams Stabilized by Partially Hydrophobic Particles

Ultralight Si₃N₄ ceramic foams have been successfully prepared through particle‐stabilized foams method, which is based on the adsorption of in situ hydrophobized Si₃N₄ particles to the liquid/air interface of the foams. Here, we firstly used a long‐chain surfactant cetyltrimethylammonium chloride to render the Si₃N₄ particles partially hydrophobic. By tailoring the surfactant concentration and pH values of the suspensions, the wet foams were stabilized to avoid coarsening and coalescence. SEM results show that the Si₃N₄ ceramic foams possess single strut walls with elongated β‐Si₃N₄ grains interlocking with each other, and their pores are uniform with an average pore size of 95 μm. The obtained ceramic foams maintain compressive strength of 1.34 ± 0.13 MPa with porosity of 92.0%, when the suspension contains 3 mmol/L surfactant at the pH of 11.0.     

The interfacial and tribological properties of Ni–Cr alloy/ceramic tribo-couples under dry sliding contact

In this paper, the tribological behaviors of Ni–Cr alloy sliding against Si₃N₄ and WC–Co at 20 °C and 600 °C were investigated on a tribometer with a ball-on-disk configuration. The experimental results indicated that Ni–Cr alloy sliding against WC–Co exhibited higher wear resistance than that sliding against Si₃N₄. From the viewpoints of the interfacial interactions between metal and ceramic (chemical reaction, wetting, adhesion, transference), the wear mechanisms were elucidated. The tribological behaviors of Ni–Cr alloy/ceramic tribo-couples were well correlated with the interfacial characteristics, namely the reactive interface and the non-reactive interface. Ni–Cr alloy/Si₃N₄ tribo-couple showed severe adhesive wear as a result of the interfacial reaction between Ni and Si₃N₄, while the non-reactivity of Ni/WC interface is the most important factor corresponding to the moderate adhesive wear in Ni–Cr alloy sliding against WC–Co. Finally, the relations among the interfacial characteristics, wear behavior, and temperature were discussed. The results may provide some experimental evidences on the design and optimization of metal/ceramic tribo-couples.     

Microstructure and reaction phases in Si3N4/Si3N4 joint brazed with Cu–Pd–Ti filler alloy

Si₃N₄ ceramic was self-jointed using a filler alloy of Cu–Pd–Ti, and the microstructure of the joint was analyzed. By using a filler alloy of Cu76.5Pd8.5Ti15 (at.%), a high quality Si₃N₄/Si₃N₄ joint was obtained by brazing at 1100–1200 °C for 30 min under a pressure of 2 × 10⁻³ MPa. The microstructure of the Si₃N₄/Si₃N₄ joint which was observed by EPMA, XRD and TEM, and the results indicated that a reaction layer of TiN existed at the interface between Si₃N₄ ceramic and filler alloy. The center of the joint was Cu base solid solution containing Pd, and some reaction phases of TiN, PdTiSi and Pd₂Si found in the Cu [Pd] solid solution.     

Application of asymmetric Si3N4 hollow fiber membrane for cross-flow microfiltration of oily waste water

The asymmetric morphology of silicon nitride (Si₃N₄) ceramic hollow fiber membrane with a selective spongiform outer layer was optimized by the air gap distance and the internal rate of coagulate for oil/water emulsion microfiltration. The effect of trans-membrane pressure (TMP), feed flow rate (FFR), and pH of the feeding emulsion on the separation performance were determined experimentally. Membrane fouling has increased by dissociation of oil droplets during filtration at high TMP and FFR values. Fouling phenomena were studied based on standard pore blocking model. The pH by affecting the surface charge of the Si₃N₄ hollow fibers and zeta potential of the feed emulsion has also been introduced as a prominent influential factor on separation efficiency. The highest values of permeate flux (390 Lm^?2h^-1) and oil rejection (95%) were recorded in alkaline pH. The fabricated Si₃N₄ ceramic membranes were completely recovered (≤99%) by simple thermal treatment at 400 °C.     

Effects of interface bonding properties on cyclic tensile behavior of unidirectional C/Si3N4 and SiC/Si3N4 composites

In this paper, the effect of fiber/matrix interface bonding properties on the cyclic loading/unloading tensile stress?strain hysteresis loops of 2 different ceramic‐matrix composites (CMCs), ie, C/Si₃N₄ and SiC/Si₃N₄, has been investigated using micromechanical approach. The relationships between the damage mechanisms (ie, matrix multicracking saturation, fiber/matrix interface debonding and fibers failure), hysteresis dissipated energy and internal frictional damage parameter have been established. The damage evolution processes under cyclic loading/unloading tensile of C/Si₃N₄ and SiC/Si₃N₄ composites corresponding to different fiber/matrix interface bonding properties have been analyzed through damage models and interface frictional damage parameter. For the C/Si₃N₄ composite with the weakest fiber/matrix interface bonding, the composite possesses the lowest tensile strength and the highest failure strain; the hysteresis dissipated energy increases at low peak stress, and the stress?strain hysteresis loops correspond to the interface partially and completely debonding. However, for the SiC/Si₃N₄ composite with weak interface bonding, the composite possesses the highest tensile strength and intermediate failure strain; and the hysteresis dissipated energy increases faster and approaches to a higher value than that of composite with the strong interface bonding.     

RF MEMS capacitive switch with leaky nanodiamond dielectric film

RF MEMS capacitive switches using leaky nanodiamond as a dielectric film are studied and compared with those using Si₃N₄. Characteristics of dielectric charging and discharging are analyzed at temperature ranging from − 196 °C to 150 °C. Electrical resistivity of leaky nanodiamond is measured to be lower than that of Si₃N₄ by 3 to 6 orders of magnitude at room temperature. Trapped charges in leaky nanodiamond dielectric discharge much more quickly than those in Si₃N₄ while the power dissipation of nanodiamond based switches remains low. As a result, charge trapping induced shift in electrostatic actuation voltage is greatly reduced compared to that with Si₃N₄ and becomes non-detectable under the reported conditions. RF MEMS capacitive switches based on leaky nanodiamond dielectric are, therefore, more reliable than those with Si₃N₄.     

Preparation and properties of silicon nitride-phosphate composites for application in microwave furnace

Si₃N₄ ceramic is one of the most promising microwave metallurgy furnace materials because of the outstanding mechanical, relatively low dielectric properties and excellent thermal shock resistance. However, the difficult sintering of Si₃N₄ ceramics extremely restrict their large-scale application in the field of refractories for microwave metallurgy. In this work, silicon nitride-phosphate ceramics were fabricated by introducing aluminum phosphate or chromium phosphate aluminum into Si₃N₄ ceramics at 1500 °C. The effect of the amount of aluminum phosphate and chromium phosphate aluminum on sintering performance and dielectric properties was investigated. The results showed that the addition of aluminum phosphate or chromium phosphate aluminum could promote sintering, and the mechanical and dielectric properties of Si₃N₄ ceramics were efficiently improved. The Si₃N₄-aluminum phosphate composites exhibited better sintering performance (higher density and mechanical property) than that of Si₃N₄-chromium phosphate aluminum composites. Meanwhile, the dielectric constant and dielectric loss of Si₃N₄-chromium phosphate aluminum composites were better than Si₃N₄-chromium phosphate aluminum composites.