High-strength and wave-transmitting Si3N4–Si2N2O-BN composites prepared using selective laser sintering

In this study, high-strength and wave-transmission silicon nitride (Si₃N₄) composites were successfully developed via selective laser sintering (SLS) with cold isostatic pressing (CIP) after debinding and before final sintering, and the optimal moulding process parameters for the SLS Si₃N₄ ceramics were determined. The effects of the sintering aids and secondary CIP on the bulk density, porosity, flexural strength, fracture toughness, and wave-transmitting properties of the Si₃N₄ composites were studied. The results showed that the increased CIP pressure was beneficial to the densification of SLS Si₃N₄ ceramics and improved their mechanical properties. However, the wave-transmitting performance decreased as the CIP pressure increased. The Si₃N₄ ceramics prepared by the moulding of sample S₁₁ were more in line with the performance requirements of the radomes. To obtain good comprehensive performance, an additional 3% of interparticle Y₂O₃ was added to the pre-printed mixed powder of granulated Si₃N₄ particles and resin and the secondary CIP pressure was adjusted to 280 MPa. After sintering, the bending strength, fracture toughness, and dielectric constant of the Si₃N₄ ceramics were 651 MPa, 6.0 MPa m^1/2, and 3.48 respectively. This study provides an important method for preparing of Si₃N₄ composite radomes using SLS process.     

Effects of AlN inorganic binder on the properties of porous Si3N4 ceramics prepared by selective laser sintering

Porous Si₃N₄ ceramics are widely used in the aerospace field due to its lightweight, high-strength, and high wave transmission. Traditional manufacturing methods are difficult to fabricate complex structural and functional ceramic parts. In this paper, selective laser sintering (SLS) technology was applied to prepare porous Si₃N₄ ceramics using AlN as an inorganic binder. And the effects of AlN content on the properties of the obtained ceramic samples were explored. As the AlN content increased, nano-Al₂O₃ and nano-SiO₂ formed the eutectic liquid phase, enhancing the sintering densification and phase transformation of Si₃N₄ poly-hollow microspheres (PHMs). The island-like partial densification structures in Si₃N₄ green bodies increased. During the high-temperature sintering, the eutectic liquid phase partially transformed into the mullite phase or reacted with AlN and Si₃N₄ to form the Sialon phase. With the increase of AlN content, the fracture mode of Si₃N₄ ceramics changed from fracturing along PHMs to fracturing across PHMs. The bonding depth between PHMs increased and the connection between the grains was tighter, so the Si₃N₄ ceramics became denser. With the increase of AlN addition, the total porosity of the porous Si₃N₄ ceramics tended to decrease and the flexural strength gradually increased. When AlN content was 20 wt%, the total porosity and the flexural strength were 33.6% and 23.9 MPa, respectively. The addition of AlN inorganic binder was carried out to develop a novel way to prepare high-performance porous Si₃N₄ ceramics by SLS.     

Preparation of Si3N4 ceramics with high strength and high reliability via a processing strategy

In this study, the preparation of Si₃N₄ ceramics with high mechanical reliability is investigated. The influences of several processing steps on the bending strength and the Weibull modulus are reported including: (i) coating of the Si₃N₄ powder with its sintering aids, (ii) oxidation of the coated powder, (iii) cold isostatic pressing, (iv) gelcasting of the green bodies and (v) gas pressure sintering. It was found that all the aforementioned steps contribute to improvements of strength and reliability of Si₃N₄ ceramics. Via an optimised processing strategy, Si₃N₄ ceramics with a bending strength and a Weibull modulus as high as 944.7±29.5 MPa and 33.9, respectively, could be prepared. Additionally, it was also found that surface modifications, i.e. coating and oxidation of Si₃N₄ powder, increased the rheological properties of the powder suspension in aqueous media, which is favourable for in situ colloidal forming such as gelcasting.     

Influence of the ratio of sintering aids on the properties of porous Si3N4 ceramics fabricated by digital light processing

The sintering aids play an important role in affecting the properties of porous Si₃N₄ ceramics. However, there are few researches on the properties of porous Si₃N₄ ceramics fabricated by digital light processing (DLP) with different ratios of sintering aids. In this paper, porous Si₃N₄ ceramics with different ratios of sintering aids (Y₂O₃-Al₂O₃) were formed by DLP technology. The influence of Y₂O₃-Al₂O₃ ratios on the properties of Si₃N₄ slurry and porous ceramic was studied systematically. The ratio of Y₂O₃-Al₂O₃ had little effect on the rheology and cure depth of Si₃N₄ slurry due to the low addition of sintering aids. The increase of Y₂O₃-Al₂O₃ ratio promoted the anisotropic growth of β-Si₃N₄. When the ratio of Y₂O₃-Al₂O₃ was 9:1, the aspect ratio of β grains reached the maximum. As the ratio of Y₂O₃-Al₂O₃ powders increased, the linear shrinkage of porous Si₃N₄ ceramics showed an increasing and then decreasing trend in three directions. When the Y₂O₃-Al₂O₃ ratio was 3:7, the shrinkage rate in the length, width and height direction reached the maximum (27.03%, 30.27% and 40.02%, respectively). The bulk density and flexural strength exhibited an initial increase followed by a subsequent decrease, while the porosity showed the opposite trend. When the Y₂O₃-Al₂O₃ ratio was 9:1, the porosity reached a maximum of 28.1%. And the bulk density and flexural strength were 2.42 g/cm³ and 421.58 MPa, respectively. This study is of great significance as it lays the experimental foundation in the performance control of porous Si₃N₄ ceramics fabricated by DLP.     

Preparation of Si3N4 ceramic based on digital light processing 3D printing and precursor infiltration and pyrolysis

The emergence of digital light processing (DLP) 3D printing technology creates favorable conditions for the preparation of complex structure silicon nitride (Si₃N₄) ceramics. However, the introduction of photosensitive resin also makes the Si₃N₄ ceramics prepared by 3D printing have low density and poor mechanical properties. In this study, high-density Si₃N₄ ceramics were prepared at low temperatures by combining DLP 3D printing with precursor infiltration and pyrolysis (PIP). The Si₃N₄ photocurable slurry with high solid content and high stability was prepared based on the optimal design of slurry components. Si₃N₄ green parts were successfully printed and formed by setting appropriate printing parameters. The debinding process of printed green parts was further studied, and the results showed that samples without defects and obvious deformation can be obtained by setting the heating rate at .1°C/min. The effect of the PIP cycle on the microstructure and mechanical properties of the Si₃N₄ ceramics was studied. The experimental results showed that the mass change and open porosity of the samples tended to be stable after eight PIP cycles, and the open porosity, density, and bending strength of the Si₃N₄ ceramics were 1.30% (reduced by 97%), 2.64 g/cm³ (increased by 43.5%), and 162.35 MPa.     

Prediction of bending strength of Si3N4 using machine learning

The bending strength of silicon nitride (Si₃N₄) plays a vital role in its application and is influenced by various process factors. Current experimental methods for investigating Si₃N₄ ceramics exhibiting low efficiency and high cost are incapable of systematically analysing the effect of process factors on the bending strength of Si₃N₄ ceramics and quantitatively predicting the optimum process parameters. In this study, machine learning (ML) approaches based on extreme gradient boosting (XGBoost) were applied to predict and analyse the bending strength of Si₃N₄ ceramics. Because the classification model of XGBoost is easily interpretable, the factors affecting the bending strength could be quantitatively evaluated. The current model can provide a suitable order of adding sintering additives to obtain excellent bending strength in Si₃N₄ ceramics. Although this study focuses on the bending strength of Si₃N₄ ceramics, the new approach reported herein is applicable for the in silico design and analysis of other ceramic materials.     

Porous Si3N4/SiC Ceramics Prepared via Nitridation of Si Powder with SiC Addition

Porous Si₃N₄/SiC ceramics with high porosity were prepared via nitridation of Si powder, using SiC as the second phase and Y₂O₃ as sintering additive. With increasing SiC addition, porous Si₃N₄/SiC ceramics showed high porosity, low flexural strength, and decreased grain size. However, the sample with 20wt% SiC addition showed highest flexural strength and lowest porosity. Porous Si₃N₄/SiC ceramics with a porosity of 36–45% and a flexural strength of 107‐46MPa were obtained. The linear shrinkage of all porous Si₃N₄/SiC ceramics is below 0.42%. This study reveals that the nitridation route is a promising way to prepare porous Si₃N₄/SiC ceramics with favorable flexural strength, high porosity, and low linear shrinkage.     

Enhanced bending strength and microwave dielectric properties of Li2MgTi3O8 ceramics by adding Si3N4 reinforcing phase

In the 5G era, the dielectric materials used in microwave electronic components must have not only have good microwave dielectric characteristics but also excellent structural characteristics. Li₂MgTi₃O₈ (LMT) ceramics have excellent microwave dielectric properties; however, their low bending strength limits their further applications in the 5G era. In this work, the dielectric properties and bending strength of LMT ceramics were optimized by the addition of Si₃N₄ reinforcing phase using a solid-phase method, and the effects of Si₃N₄ addition on the sintering properties, microscopic structure, crystalline phase, dielectric properties and bending strength of ceramics were investigated. The X-ray diffraction pattern indicates that all ceramics exhibit spinel structure. Combined with the phenomenon of grain reduction in the SEM graph, it indicates that the addition of Si₃N₄ can inhibit the grain growth and achieve the purpose of fine-grain strengthening. The dispersion enhancement of second phase particles is also one of the reasons for the increase of bending strength. LMT ceramics doped with 0.5 wt% Si₃N₄ exhibited the maximum bending strength after sintering at 1050 °C for 4 h, which was 76.97% higher than that of pure LMT ceramics. In addition, the ceramics exhibited outstanding dielectric properties: a dielectric constant of 23.20, quality factor of 49344 GHz, and temperature coefficient of ?5.90 ppm/°C. The high bending strength and good microwave dielectric properties indicate that Si₃N₄-added LMT ceramics can be effectively applied in the 5G era.     

A non-sintering fabrication method for porous Si3N4 ceramics via sol hydrothermal process

A non-sintering fabrication method for porous Si₃N₄ ceramics with high porosity and high mechanical strength was proposed. Strength of the porous ceramics can be obtained by silica sol mass transfer process in hydrothermal conditions rather than a traditionally controlled high temperature sintering process. Under hydrothermal circumstances, silica sol is continuously transferred to the necks of Si₄N₃ powder compact, depositing there and thus consolidating the ceramic skeleton. The key of the method to obtain homogeneous microstructure and mechanical strength is how to keep the silica sol from gelatin during hydrothermal procedure. The stabilization of silica sol and its affecting factors were studied. The results indicated that ultrasonic treatment makes alkali-catalyzed silica sol remain stable even in 200?℃ hydrothermal condition, which insures consecutive silica transportation. The effect of hydrothermal time on open porosity/mechanical strength of the porous Si₄N₃ ceramics were also thoroughly investigated. The porous Si₄N₃ ceramics with open porosity above 42% and flexural strength of 45?MPa were obtained without any high temperature sintering process. This method can be widely employed for the preparation of other porous ceramics as well.     

Mechanical characterization of highly porous β-Si3N4 ceramics fabricated via partial sintering & starch addition

In this study, porous β-Si₃N₄ ceramics containing limited amount of Sm₂O₃ and CaO as sintering aids were produced by addition of potato starch (10 and 20 vol.%) and partial sintering. Two different Si₃N₄ powders, α- and β-, were used as starting materials. Scanning electron microscopy investigations revealed that development of elongated β-Si₃N₄ grains were much more pronounced when α-Si₃N₄ starting powder was used. Even though porosity values of the compositions prepared by using α-Si₃N₄ (～57.0–58.4%) is significantly higher than the samples produced by β-Si₃N₄ (42.6%), no significant change was observed for the bending strength, fracture toughness and Weibull modulus. This indicates that microstructural features have a significant contribution to the mechanical properties of the porous materials in terms of bending strength and fracture toughness.     

Neural network modeling and analysis of gel casting preparation of porous Si3N4 ceramics

Based on orthogonal experimental results of porous Si₃N₄ ceramics by gel casting preparation, a three-layer back propagation artificial neural network (BP ANN) was developed for predicting the performances of porous Si₃N₄ ceramics. The results indicated that BP ANN was a very useful and accurate tool for the prediction and optimization of porous Si₃N₄ ceramics performances. By using the developed ANN model, the influences of the compositions on performances of porous Si₃N₄ ceramics were investigated, and some important conclusions were drawn as follows: for the flexural strength of Si₃N₄ ceramics, solid loading has an optimum value where can achieve a maximum value, and the optimum solid loading decreases with the increase of monomer content; the porosity of sintering body monotonically decreases with the increase of solid loading, and it increases with monomer content; the porosity of sintering body monotonically increases with the increase of the ratio of crosslinking agent to monomer.     

Pore structure control of Si3N4 ceramics based on particle-stabilized foams

Porous Si₃N₄ ceramics with open, closed pores and nest-like structures were prepared by direct foaming method, and the stability of bubbles and the microstructures of sintered Si₃N₄ foam ceramics were investigated. The bubbles produced by short-chain amphiphiles have higher stability as compared with that produced by long-chain surfactants. Si₃N₄ ceramic foams using short-chain amphiphiles are particle-stabilized one, porous Si₃N₄ ceramics with open and closed pores can be easily prepared with this method, and the nest-like microstructure in Si₃N₄ foam ceramics is achieved at high gas-pressure sintering conditions. The decrease of flexural strength due to the increase of porosity can be weakened by decreasing pore size.     

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.     

Dielectric and mechanical properties of porous Si3N4 ceramics prepared via low temperature sintering

Borophosphosilicate bonded porous silicon nitride (Si₃N₄) ceramics were fabricated in air using a conventional ceramic process. The porous Si₃N₄ ceramics sintered at 1000–1200 °C shows a relatively high flexural strength and good dielectric properties. The influence of the sintering temperature and contents of additives on the flexural strength and dielectric properties of porous Si₃N₄ ceramics were investigated. Porous Si₃N₄ ceramics with a porosity of 30–55%, flexural strength of 40–130 MPa, as well as low dielectric constant of 3.5–4.6 were obtained.     

A Novel Si3N4–SiC Ceramic Used for Volumetric Receivers

Si₃N₄–SiC composite ceramics used for volumetric receivers were fabricated by pressureless sintering of micrometer SiC, Si₃N₄, andalusite, and other minor additions powders. Mechanical, thermal expansion, thermal conductivity, and thermal shock resistance properties were tested at different sintering temperatures. The best sintering temperature of optimum formula A2 is 1360°C, and the bending strength reaches 79.60 Mpa. And moreover, its thermal expansion coefficient is 6.401 × 10^?6/°C, thermal conductivity is 7.83 W/(m K), and no crack occurs even subjected to 30 cycles thermal shock with a bending strength increase rate of 4.72%. X‐ray diffraction results show that the phase constituents of the sintered products mainly consist of SiC, Si₃N₄, mullite, and quartz. Microstructure that is most appropriate and exhibits maximal thermal shock resistance was detected using SEM. The porosity of Si₃N₄–SiC ceramic foam prepared from formula A2 is 95%, which provides a rapid and steady action for the receiver. The evaluation of the present foam shows that Si₃N₄–SiC ceramic composite is a good candidate for volumetric receivers.     

Indirect selective laser sintering of epoxy resin-Al2O3 ceramic powders combined with cold isostatic pressing

To fabricate Al₂O₃ ceramic components with complex shape, selective laser sintering (SLS) combined with cold isostatic pressing (CIP) process was used to consolidate Al₂O₃ powder with additive of epoxy resin E06 (ER06) and polyvinyl alcohol (PVA). The starting material preparation combined spray drying with mechanical mixing to formulate compound powder consisting of PVA (1.5 wt%), ER06 (8 wt%) and Al₂O₃ and provide a good fluidity for SLS. Experimental investigations were carried the shrinkage, relative density, bending strength of Al₂O₃-ER06 SLS specimens in order to optimize the laser sintering parameters. It was found that Al₂O₃-ER06 SLS specimens represented acceptable shrinkage, high density and bending strength when laser power, scanning speed, scanning space and layer thickness were, respectively, 21 W, 1600 mm/s, 100 μm and 150 μm. Following that, the SLS specimens were processed through CIP to eliminate the pores in green ceramics. Finally, the optimized SLS/CIP Al₂O₃ specimens were debinded, sintered to produce crack-free Al₂O₃ bodies. The final Al₂O₃ components achieved a relative high density of more than 92% after furnace sintering. The study shows a novel and promising approach to fabricate complex ceramic matrix and ceramic components via indirect SLS and CIP process.     

Preparation and characterization of porous Si3N4-bonded SiC ceramics and morphology change mechanism of Si3N4 whiskers

Porous Si₃N₄-bonded SiC ceramics with high porosity were prepared by the reaction-sintering method. In this process, Si₃N₄ was synthesized by the nitridation of silicon powder. The X-ray diffraction (XRD) indicated that the main phases of the porous Si₃N₄-bonded SiC ceramics were SiC, α-Si₃N₄, and β-Si₃N₄, respectively. The contents of β-Si₃N₄ were increased following the sintering temperature. The morphology of Si₃N₄ whiskers was investigated by scanning electron microscope (SEM), which was shown that the needle-like (low sintering-temperature) and rod-like (higher sintering-temperature) whiskers were formed, respectively. From low to high synthesized temperature, the highest porosity of the porous Si₃N₄ bonded SiC ceramic was up to 46.7%, and the bending strength was ~11.6?MPa. The α-Si₃N₄ whiskers were derived from the reaction between N₂ and Si powders, the growth mechanism was proved by Vapor–Solid (VS). Meanwhile, the growth mechanism of β-Si₃N₄ was in accordance with Vapor–Solid–Liquid (VSL) growth mechanism. With the increase of sintering temperature, Si powders were melted to liquid silicon and the α-Si₃N₄ was dissolved into the liquid then the β-Si₃N₄ was precipitated successfully.     

Effects of different types of sintering additives and post-heat treatment (PHT) on the mechanical properties of SHS-fabricated Si3N4 ceramics

Porous silicon nitride (Si₃N₄) ceramics were fabricated by self-propagating high temperature synthesis (SHS) using Si, Si₃N₄ and sintering additive as raw materials. Effects of different types of sintering additives with varied ionic radius (La₂O₃, Sm₂O₃, Y₂O₃, and Lu₂O₃) on the phase compositions, development of Si₃N₄ grains and flexural strength (especially high-temperature flexural strength) were researched. Si₃N₄ ceramics doped with sintering additive of higher ionic radius had higher average aspect ratio, improved room-temperature flexural strength but degraded high-temperature flexural strength. Besides, post-heat treatment (PHT) was conducted to crystallize amorphous grain boundary phase thus improving the creep resistance and high-temperature flexural strength of SHS-fabricated Si₃N₄ ceramics. Excellent high-temperature flexural strength of 140 MPa~159 MPa and improved strength retention were achieved after PHT at 1400 °C.     

Thermal shock behavior of porous Si3N4 ceramics with Nd2O3 as sintering additive

The thermal shock behavior of porous Si₃N₄ ceramics with Nd₂O₃ as sintering additive was investigated by the water quenching method in the temperature difference range from 200 to 1500°C. The porosity and residual flexural strength of the specimens after single water quenching were measured to reveal the influence of thermal shock on porous Si₃N₄ ceramics. It was found that the critical temperature was 780°C, which was almost 230°C higher than its dense counterpart reported by other researchers. Scanning electron microscope was used to examine the microstructure evolution of the external surface and interior after water quenching. Surface oxidation and cracks formation were found to be the primary cause of the strength degradation of porous Si₃N₄ ceramics. The phase composition variation in the surface was also characterized by X-ray diffraction.     

Mechanical property and gas filtration behavior of porous reaction bonded Si3N4 with monodispersed PMMA as pore former

Porous Si₃N₄ ceramics were prepared by gel casting combined with a reaction bonding route using monodispersed PMMA as the pore former, and Isobam was used as a gel agent. With the PMMA addition varying from 0 to 20 wt.%, the bending strength was degraded from 94.0 to 39.1 MPa owing to the increased porosity and decreased bulk density. The β-Si₃N₄ prismatic grains and round pores introduced by the monodispersed PMMA micro balls would endow the samples with high strength, and the permeability of the resulting samples was increased obviously with the increase of PMMA addition. Flue gas filtration test exhibited that the filtration efficiency of the porous ceramics filter was not degraded with introducing of the PMMA pore former, even though the permeability was increased obviously. The block type of the sample with 20-wt.% PMMA additions during filtration was cake filtration, which indicates that the sample has the characteristic of being reusable after back-blowing in flue gas filtration applications. Porous Si₃N₄ with high strength and permeability fabricated via the reaction bonding route exhibits great potential for low-cost high-performance ceramics filters.