Fabrication processing and mechanical properties of Si3N4 ceramic turbocharger wheel

A composite technique was chosen to fabricate Si₃N₄ ceramic turbine wheel based on modified investment casting (MIC), slip casting (SP) and mold constraint hot isostatic pressing (MCHIP) aided by a near-net dimension using the gypsum mold and multi-piece Y₂O₃ ceramic mold. The detailed fabrication processing of Si₃N₄ ceramic turbine wheel was described. And the flexural strength and fracture toughness after different work temperature and speed were discussed. The results showed that owing to occurrence of phase transformation and chemical reaction, excess temperature resulted in interface cracking and interface debonding, flexural strength and fracture toughness decrease. Thermal expansion and centrifugal force under excessive high speed brought many pores in the microstructure and resulted in crack initiation and crack propagation. The critical work temperature was 700?°C and critical work speed was 100,000 r/min, which were obtained from the test and simulation results.     

Effect of the molecular weight and concentration of PEG solution on microstructure and mechanical properties of Si3N4 ceramics fabricated by gel-casting

Gel-casting is a promising preparation technology of Si₃N₄ structural ceramics. The process involves drying of the “green” gel-cast parts before densification. And the drying of green gel-cast bodies is an important step in the gel-casting manufacturing process. In this work, the Si₃N₄ gel-cast green bodies were dried in polyethylene glycol (PEG) solution with the purpose of obtaining Si₃N₄ ceramics with good mechanical properties. The effect of the molecular weight and concentration of PEG solution on drying rate, microstructure and mechanical properties of Si₃N₄ ceramics was studied. The results indicated that with the increase of molecular weight of PEG, the drying rate increased obviously and the structure became more uniform and dense when the concentration of solution was 20?wt%. The Si₃N₄ ceramics after sintering have the excellent flexural strength (662.6?MPa) under PEG600 drying condition. Furthermore, the concentration of PEG600 solution had a positive effect on drying and sintering of the green body. Therefore, the bending strength reached 871.1?MPa under 65?wt% PEG 600 solution drying condition. Overall, the drying process (drying in 65?wt% PEG600 solution) promotes the efficiency and quality of drying of Si₃N₄ gel-cast green bodies, which is beneficial for the subsequent drying and sintering process.     

Grain growth in microwave sintered Si3N4 ceramics sintered from different starting powders

Silicon nitride ceramics have been produced by microwave sintering at 28 GHz with Y₂O₃, Al₂O₃ and MgO as sintering additives. The effect of initial β content of the Si₃N₄ starting powder on the microstructural development has been assessed by scanning electron microscopy (SEM) and quantitative image analysis. Phase transformation behaviour was assessed by X-ray diffraction. Mechanical properties of the sintered bodies were determined through assessment of hardness and fracture toughness. It was found that the samples sintered from powders with lower initial β content developed larger grains than those from higher β content powders, due to fewer nucleation sites during the →β transformation. However, attempts to develop a more bimodal microstructure by using a mixture of the two grades of powder, in an effort to increase both fracture toughness and fracture strength, were unsuccessful. In this case the microstructure was similar to that developed in the materials produced from higher β content powders. The mechanical properties of the sintered bodies were very similar, despite differences in microstructure. This was attributed to the strong bonding between the grains and grain boundary phase resulting in crack paths in all the materials that were predominantly transgranular, with little debonding or crack deflection. Under these circumstances the effect of larger grains is eliminated.     

Effect of carboxymethyl cellulose addition on the properties of Si3N4 ceramic foams

The effect of carboxymethyl cellulose (CMC) addition on the preparation of Si₃N₄ ceramic foam by the direct foaming method was investigated. The addition of CMC in the foam slurry can reduce the surface tension, increase the viscoelasticity of foams, and improve their stability and fluidity. The foam ceramics show low shrinkage during drying owing to the CMC and the gelation of acrylamide monomers. The surface structure of dried foam is uniform, and there are no macropores and cracks on the surface. The sintered Si₃N₄ foam ceramics have very uniform pore distribution with average pore size of about 16 μm; the flexure strength is as high as 3.8–77.2 MPa, and the porosity is about 60.6–82.1%.     

Fabrication and properties of porous Si3N4 ceramics by aqueous gelcasting using low-toxic DMAA gelling agent

A low-toxic and water-soluble monomer N, N-dimethylacrylamide (DMAA) was employed as a gelling agent in the gelcasting of porous Si₃N₄ ceramics. The process conditions and composition for slurry preparation (with a solid loading of 36?vol%), the consolidation and sintering of green bodies were investigated and optimized. The effects of various factors such as zeta potential, pH value of the premix solution, dispersant dosage and ball milling time on the rheological properties of the slurries were investigated. The results suggest that the best rheological properties (66.5 mPa.s at a shear rate of 96.3?s^?1) of the slurries were obtained when pH value ranged between 9 and 11, dispersant dosage reached 1?wt%, and ball milling time was 6?h. All the as-prepared green bodies showed a homogeneous microstructure and high flexural strength ≥ 26?MPa with a maximum up to 46.3?MPa when the ratio of DMAA to MBAM, initiator dosage, polymerization temperature and time were 14, 1?wt%, 70?°C and 90?min, respectively. The sintered bodies had a homogeneous microstructure, excellent and regulatable properties, a flexural strength of 216.3–327.3?MPa, and a porosity of 39.6–29.1% by varying the sintering temperature from 1710?°C to 1810?°C and the holding time from 1?h to 3?h. The superior comprehensive effect makes DMAA a promising candidate for an environmentally friendly gelling agent in gelcasting of porous Si₃N₄ ceramics.     

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).     

Effects of Zn2SiO4 on the phase evolution,thermal expansion and mechanical properties of LiAlSiO4 ceramic

LiAlSiO₄ (abbreviated as LAS) ceramics doped with variable mass percent of Zn₂SiO₄ were prepared by conventional solid-state route. The effects of Zn₂SiO₄ on the phase evolution, microstructure, thermal expansion and mechanical properties have been fully investigated. The results show that Zn₂SiO₄ reacted with LAS matrix to produce Li₂Al₂Si₃O₁₀ and ZnAl₂O₄. Fine-grain ZnAl₂O₄ phase accumulated on the grain boundaries of the main phase, which was helpful to improve the density. Simultaneously, both of the flexure strength and Vickers hardness of the multiphase ceramics were significantly enhanced with the increasing mass percent of Zn₂SiO₄ for the reason of dispersion strengthening effect. In addition, when the content of Zn₂SiO₄ increased from 10?wt% to 22.5?wt%, the coefficient of thermal expansion (CTE) of the composite ceramics increased monotonously from ??5.24?×?10^?6/K to 1.49?×?10^?6/K. Typically, the LAS ceramic doping with 17.5?wt% Zn₂SiO₄ sintered at 1175?°C for 4?h possesses excellent properties: α?=?0.65?×?10^?6/K, H_v =?5.34?GPa, σ_s =?102.6?MPa, which is a promising material in laser gyroscope and precision machining fields.     

Enhanced toughness and reliability of Si3N4-SiCw composites under oscillatory pressure sintering

We reported an oscillatory pressure sintering (OPS) process to consolidate Si₃N₄-SiCw composites. For comparison, the composites were also prepared by hot pressing (HP) method. The specimen by OPS process reveals an accelerated rate of grain growth in the c axial direction and thus an increased average aspect ratio compared with the specimen by HP process. The oscillatory pressure also performs a positive impact on the Si₃N₄-SiCw composites as the bulk density of the OPS specimen increases to 3.270?g?cm^?3 accompanied with higher fracture strength and hardness of 1133?MPa and 16.1?GPa, respectively, compared with those of the HP specimen. Significantly, the increased fracture toughness and Weibull modulus found in the OPS specimen indicate toughening effects and material reliability are improved aided by the oscillatory pressure. Current results suggest OPS to be a promising technique for preparing highly densified Si₃N₄-SiCw composites with enhanced mechanical properties.     

Laser surface nanostructuring for reliable Si3N4/Si3N4 and Si3N4/Invar joined components

IR pulsed laser radiation in air was applied to Si₃N₄ and Invar to obtain reliable Si₃N₄/Si₃N₄ and Si₃N₄/Invar adhesive bonded components. The laser pre-treatment produced a homogeneous nanostructured oxide layer on the surfaces, which effectively increased the adhesion at the adhesive/adherends interface and led to cohesive failure in the joining material. The mechanical strength of Si₃N₄/ Si₃N₄ and Si₃N₄/Invar joined components was measured, with and without laser nanostructuring, before and after thermal cycling from room temperature to 50?K, and it resulted that the exposure to extremely low temperatures did not affect the mechanical integrity of the joints. It was also demonstrated that this laser pre-treatment did not alter the mechanical properties of the ceramic substrate.     

Effect of sodium polyacrylate on mechanical properties and microstructure of metakaolin-based geopolymer with different SiO2/Al2O3 ratio

The mechanical properties and microstructure of geopolymer are affected by the molar ratio of SiO₂/Al₂O₃. Meanwhile, organic polymer has the effect of improving the toughness of geopolymer, which depends on the SiO₂/Al₂O₃ ratio of geopolymer inevitably. Therefore, it is important to investigate the effect of the organic polymer on the mechanical properties and microstructure of geopolymer with varying SiO₂/Al₂O₃ ratio for using organic polymer to modify geopolymer. In this work, the SiO₂/Al₂O₃ ratios of metakaolin-based geopolymers are adjusted to 2.0, 2.5, 3.0, 3.5 and 4.0 by adding silica fume and β-Al₂O₃, with Na₂O/SiO₂, H₂O/SiO₂ being maintained at 0.2, 4.0, respectively. The geopolymers with each SiO₂/Al₂O₃ ratios are modified by addition of 0, 0.4, 0.8, 1.2 and 1.6?wt% of sodium polyacrylate (PAAS).The mechanical properties of these samples are measured and the rate of change is used to characterize the effect of PAAS on the metakalin-based geopolymers. The mechanism is also shown by 29Si NMR, XPS and FTIR. The results show that the effects of polymer on the mechanical properties of metakaolin-based geopolymer are affected by SiO₂/Al₂O₃ ratio and the effect becomes less obvious with SiO₂/Al₂O₃ ratio increasing from 2.0 to 4.0. Incorporation of PAAS can reduce the degree of polymerization of [SiO]₄ or [AlO]₄ in geopolymer and form the Si?O?C bond, which are two main reasons for polymer improving the toughness of geopolymer. But these effects decrease when the SiO₂/Al₂O₃ ratio of geopolymer increases from 2.0 to 4.0, which is corresponding to the effect on the mechanical properties. The toughening effect of organic polymer on geopolymer depends on the SiO₂/Al₂O₃ ratio of geopolymer, and only the geopolymer with lower SiO₂/Al₂O₃ ratio (no more than 2.5 in this work) can be significantly toughening modified by organic polymer. Therefore, it is necessary to consider the SiO₂/Al₂O₃ ratio of the geopolymer when geopolymer modified by organic polymer is designed.     

A novel aerogels/porous Si3N4 ceramics composite with high strength and improved thermal insulation property

A novel ZrO₂-SiO₂ aerogels/porous Si₃N₄ ceramics composite with high strength, low density, good dielectric properties and low thermal conductivity was synthesized by filling ZrO₂-SiO₂ aerogels into the porous Si₃N₄ ceramics through vacuum sol-impregnating. The effects of aerogels on the microstructure and properties of composite were discussed. The results show that aerogels could form a mesoporous structure and significantly decrease the thermal conductivity from 9.8 to 7.3 W m^?1 K^?1. Meanwhile, the density, mechanical and dielectric properties of the porous Si₃N₄ ceramics could not be affected after introducing ZrO₂-SiO₂ aerogels. The composite exhibits high porosity (62.6%), high flexural strength (53.86 MPa) and low dielectric constant (2.86). The ZrO₂-SiO₂ aerogels/porous Si₃N₄ ceramics composite shows great potential as radome materials applied in the fields of aerospace.     

Microstructure and mechanical properties of Nb4AlC3 MAX phase synthesized by reactive hot pressing

The present study aims at synthesizing the Nb₄AlC₃ MAX phase by reactive hot pressing using Nb:Al:NbC as starting materials. In order to identify the reaction path, interrupted tests at intermediate temperatures were performed as well as differential thermal analyses (DTA) of powders. Coupling between DTA and XRD data and SEM/EDS analyses of the samples allows a better understanding of the reaction mechanisms. Pure and fully dense Nb₄AlC₃ samples were obtained and characterized for the first time by EBSD and SEM to assess, using an original method, grain size and microstructure. For instance, in the present study, an average grain length of 5–7?µm was obtained.Standard mechanical characterizations showed interesting properties: K_Ic≈?6?MPa?m^1/2, E?≈?350?GPa and α?≈?7.10^?6 °C^?1. Oxidation performance of Nb₄AlC₃ was evaluated at 1100?°C under cyclic conditions. A breakaway regime was instantaneously established for this condition, thus demonstrating the impossibility of using such an unprotected material for structural applications at high temperature in air environment.     

High temperature mechanical properties of porous Si3N4 prepared via SRBSN

The high temperature strength and fracture behavior of porous Si₃N₄ ceramics prepared via reaction bonded Si₃N₄ (RBSN) and sintered reaction bonded Si₃N₄ (SRBSN) were investigated at 800–1400?°C. The weight gain after oxidation for 15?min and the microstructure of the edge and center of the fracture surface clearly show that the internal oxidation of porous SRBSN is unavoidable with porosity of ~ 50% and mean pore size of 700?nm. The oxidation of Si₃N₄ and intergranular Y₂Si₃O₃N₄ phase may responsible for the high temperature strength degradation of SRBSN. Porous Si₃N₄ ceramics prepared with addition of 1?wt% C showed low strength degradation at temperature >?1200?°C.     

Fabrication,microstructure and mechanical properties of co-continuous TiCx/Cu-Cu4Ti composites prepared by pressureless-infiltration method

The co-continuous TiC_x/Cu-Cu₄Ti composites were prepared by infiltrating melting Cu into TiC_0.5 porous preforms. TiC_0.5 porous preforms were firstly synthesized by in-situ solid reaction process using powder Ti and carbon black as the starting materials, PVB as shaping and pore-forming agent. The prepared TiC_0.5 preforms showed 3D-connected visible pores characterized with two classes of sizes, i.e. intergranular pores with size of 10–30?µm and intracrystalline pores with 2–3?µm. Microstructure and phase compositions of the composites were detected by scanning electron microscopy (SEM) equipped with EDS and X-ray diffraction (XRD). Metal region of the composites contained Cu as well as a new phase Cu₄Ti, which was formed by reaction of Cu and TiC_0.5. Composites prepared by this method had a compact structure and strong interface. Meanwhile, metal phase and ceramic phase maintained a co-continuous structure in three dimensions. Cu-Cu₄Ti entered into the TiC_x ceramic particles like root structure during the infiltration process. Flexural strength, fracture toughness and Vickers hardness of the composites reached 948.20?±?124.04?MPa, 12.62?±?0.37?MN?m^?3/2 and 606.4?±?36.7 respectively when content of TiC_x was 71.22?vol%.     

Microstructure and properties of BN/Si3N4 composites with addition of microwave synthesized Y2O3-MgO nanopowders

Y₂O₃-MgO nanocomposite powder was synthesized by a microwave technique and doped into gas-pressure sintered BN/Si₃N₄ composites to acquire a highly wave-transparent material that could be utilized in spacecrafts. The XRD and SEM analyses indicated that the main phases were rod-like β-Si₃N₄ particles and MgSiO₃. In this case, a BN/Si₃N₄ ceramic with 8?wt% Y₂O₃-MgO nanopowder displayed a density of 2.5?g/cm³. The permittivity and transmission efficiency were approximately 4.6% and 71.4%, respectively, at frequencies of 8.2–12.4?GHz, which achieved the best overall wave-transparent performance. The porosity of the material in combination with the inclusion of the boron nitride component creates a synergistic effect that appears to contribute to wave-transparent efficiency.     

Quantitative analysis of toughening effect of crack deflection on Si3N4/Si2N2O composites through improved indentation method

In this study, Si₃N₄/Si₂N₂O composite ceramics prepared by hot pressing were used as an example, and the material fracture morphology and fracture mechanism were analyzed. Based on the formula of fracture toughness measured by an indentation method, a quantitative computation method was proposed to determine the toughened effect of ceramic materials resulting from the crack deflection by the second phase. The grain size and sintering density are increased with the increase of sintering temperature. The toughening effects resulting from the crack deflection is increased, and the main mode of fracture is transformed into the transgranular fracture. The Si₂N₂O grains can play a role in the toughening process because these grains can hinder the cracks extending along the radial direction. However, when the cracks extend in the axial direction, the toughening effect of Si₂N₂O grains is not obvious because of the internal stacking faults in the axial direction. The improved indentation method can quantitatively analyze the toughening effect of the second phase of composite ceramics, and the validity of this method are verified by comparing the fracture toughness of Si₃N4/Si₂N₂O and fine grained β- Si₃N₄ ceramics.     

Microstructure and mechanical properties of Si3N4f/Si3N4 composites with different coatings

The Si₃N₄ coating and Si₃N₄ coating with Si₃N₄ whiskers as reinforcement (Si₃N_4w-Si₃N₄) were prepared by chemical vapor deposition (CVD) on two-dimensional silicon nitride fiber reinforced silicon nitride ceramic matrix composites (2D Si₃N_4f/Si₃N₄ composites). The effects of process parameters of as-prepared coating including the preparation temperature and volume fraction of Si₃N_4w on the microstructure and mechanical properties of the composites were investigated. Compared with Si₃N₄ coating, Si₃N_4w-Si₃N₄ coating shows more significant effect on the strength and toughness of the composites, and both strengthening and toughening mechanism were analyzed.     

Polysilazane derived micro/nano Si3N4/SiC composites

The pyrolised polysilazanes poly(hydridomethyl)silazane NCP 200 and poly(urea)silazane CERASET derived Si–C–N amorphous powders were used for preparation of micro/nano Si₃N₄/SiC composites by hot pressing. Y₂O₃–Al₂O₃ and Y₂O₃–Yb₂O₃ were used, as sintering aids. The resulting ceramic composites of all compositions were dense and polycrystalline with fine microstructure of average grain size <1 μm of both Si₃N₄ and SiC phases. The fine SiC nano-inclusions were identified within the Si₃N₄ micrograins. Phase composition of both composites consist of , β modifications of Si₃N₄ and SiC. High weight loss was observed during the hot pressing cycle, 12 and 19 wt.% for NCP 200 and CERASET precursors, respectively. The fracture toughness of both nanocomposites (NCP 2000 and CERASET derived) was not different. Indentation method measured values are from 5 to 6 MPa m^1/2, with respect to the sintering additive system. Fracture toughness is slightly sensitive to the SiC content of the nanocomposite. Hardness increases with the content of SiC in the nanocomposite. The highest hardness was achieved for pyrolysed CERASET precursor with 2 wt.% Y₂O₃ and 6 wt.% Yb₂O₃, HV 23 GPa. This is a consequence of the highest SiC content as well as the chemical composition of additives.     

Joining of Si3N4/Si3N4 with in-situ formed Si-Al-Yb oxynitride glasses interlayer

Si₃N₄ ceramic was successfully joined to itself with in-situ formed Yb-Si-Al oxynitride glass interlayer. The joints were composed of three parts: (I) Si₃N₄ matrix, (II) oxynitride glass interlayer in which hexagonal or fine elongated β-sialon grains and a few ball-like β-Si₃N₄ grains exist, and (III) diffusion zone in Si₃N₄ matrix containing a thin dark layer and a ~ 25?µm thick bright layer. The seam owned similar microstructure to matrix and was inosculated with the matrix as a whole. The strength of the joint tended to increase with the increase of bonding temperature and reached the value of 225?MPa, when the joints were prepared at 1600?°C for 30?min under a pressure of 1.5?MPa. The high-temperature strength remained 94.7% and 75.2% of R.T. strength when the joints were tested at 1000?°C and 1200?°C, respectively. It may be contributed to the high softening temperature of the Yb-Si-Al oxynitride glass phase formed in the seam. Even suffered to the air exposure for 10?h at 1200?°C, the residual strength of the joints was still 143?MPa, attributed to the existence of YbAG phase.     

Porous (SiCw-Si3N4w)/(Si3N4-SiC) composite with enhanced mechanical performance fabricated by 3D printing

SiC whisker and Si₃N₄ whisker-reinforced Si₃N₄-SiC ((SiC_w-Si₃N_4w)/(Si₃N₄-SiC)) composite was synthesized by 3D printing for the first time, by the combination of printed-Si-body nitridation and chemical vapor infiltration-SiC methods. The mechanical properties of the composite could be optimized through the adjustment of SiC_w content and load direction. A SiC_w content of 3?wt% was found to be the optimal scheme, and accordingly, the average bulk density increased by 22.4%, the bending strength increased by 63.6%, the compressive strength parallel to the printing layer increased by 404.8%, and the compressive strength perpendicular to the printing layer increased by 157.1%, compared with the bulks without whiskers. The enhanced mechanical performance was mainly attributed to the process of densification by CVI, and the effect of the homogeneous whiskers bridging, pull-out and deflecting crack to expend energy. The achieved indices meet the requirements for 3D-printed porous ceramic matrix composite targeted for commercial and military field applications.