A high-safety lithium-ion battery electrospun separator with Si3N4-assisted sulfonated poly(ether ether ketone) for regulating lithium flux.

The uncontrolled lithium (Li) dendrite growth significantly impacts the safety performance of polymer separators. To mitigate this growth, this study introduces Si3N4 into sulfonated poly(ether Ether Ketone) (SPEEK) and prepares Si3N4/SPEEK composite separators via electrospinning. At the interface between the Si3N4/SPEEK separator and the Li anode, the Si nanowires that form impede Li dendrite growth, thereby enhancing the electrochemical performance of lithium-ion batteries (LIBs). The Li deposition test of the 10 % Si3N4/SPEEK separator can operate for 1000 h without short-circuiting. Additionally, the LiFePO4||Li cell with the 10 % Si3N4/SPEEK separator shows improved initial discharge capacity (157.8 mAh g-1 at 1C) and superior rate performance (125 mAh g-1 at 10C). Moreover, the nano-scale Si3N4 endows the separator with robust thermal and mechanical properties. The FLIR observations reveal that the 10 % Si3N4/SPEEK separator maintains uniform thermal distribution and structural integrity even at 300 °C, ensuring safe battery operation at high temperatures. The additional load of the 10 % Si3N4/SPEEK separator can reach 10.2 mN, which enhances the puncture resistance of the separator. This work provides a solid approach for the application of SPEEK as a high-safety and high-rate LIB separator.

Production and characterization of low-density silicon nitride reinforced zinc nanocomposite coatings on mild steel for applications in marine and automotive industries.

In today's automotive, marine and petrochemical industries, the desire for lightweight materials has increased. Hence, necessitating the production of components with low density. In this work, lightweight Zn-Si3N4 coatings were developed by including Si3N4 in the zinc matrix. The optimal coatings were produced on steel samples at 45 °C and varied Si3N4 particles and voltages following ASTM A53/A53M standard. The deterioration (corrosion) property i.e. corrosion rate (CR) and current density (jocorr) of the uncoated (control) and coated samples were examined in 0.5 M of sulphuric acid using a potentiodynamic polarization technique following ASTM G3/G102 standard. The microstructure of the samples was studied via the SEM micrographs and XRD patterns, while the wear performance resistance (following ASTM G99 standard) and electrical conductivity of the samples were examined with a pin-on-disc tribometer and ammeter-voltmeter. The corrosion experiment indicated that the uncoated mild steel specimen possessed a CR of 12.345 mm year-1 and jocorr of 1060 µA/cm2, while the CR and jcorr of the coated samples ranged from 2.6793 to 4.7975 mm year-1 and 231-413 µA/cm2, respectively. The lower CR and jcorr values of the coated specimens, relative to the coated sample showed that the coatings possessed superior passivation ability in the test medium. The SEM micrographs of the samples showed refined morphology, while the XRD patterns revealed high peak intensity crystals such as Zn4SiN, ZnNSi, Zn4N and Zn2NSi, which could be beneficial to the mechanical properties and corrosion resistance of the steel. Moreover, the wear resistance study indicated that the COF of the uncoated sample ranged from 0.1 to 0.5, while those for coated specimens ranged from 0.05 to 0.35. Similarly, the uncoated steel exhibited a wear volume (WV) of 0.00508 mm3, while the WV of the coated specimens ranged from 0.00266 to 0.0028 mm3, indicating the existence of high strengthening mechanisms between the interface of the protecting device and the steel. Also, the electrical conductivity of the mild steel sample reduced from 12.97 Ω-1cm-1 to 0.64 Ω-1cm-1, indicating that the electrical resistivity of the steel was enhanced by the coatings.

Tailoring thermal transport and confinement effect of GaN/Si3N4nanowires utilizing core-shell architecture.

The thermal transport properties of nanowires (NWs) can be significantly influenced by the implementation of a core-shell structure, which introduces interface scattering and phonon localization effects, opening avenues for novel applications. In this paper, we use the method of non-equilibrium molecular dynamics to simulate the effects of system temperature, cross-sectional width, and nanopillar interface on the thermal transport of GaN/Si3N4core-shell NWs. The thermal transport process of phonons in core-shell NWs is studied by calculating the vibrational density of states, phonon participation rate, and dispersion curve. The results show that the core-shell NWs characterized by smooth interfaces exhibit a 17.4% decrease in thermal conductivity (TC) at room temperature when contrasted with pristine GaN NWs. Furthermore, the TC of GaN/Si3N4core-shell NWs can be further reduced by adding nanopillars at the interface. Due to resonance effect, thus effectively regulating the thermal transport. The presence of nanopillars increases phonon-surface scattering intensity at low-frequency and modifies phonon dispersion to decrease the group velocity. In addition, the hybridization of phonon modes between those of the nanopillars and the Si3N4shell gives rise to numerous dispersionless resonance phonon modes that span the entire phonon spectrum. This research delves into the effects of nanopillars and interfaces on thermal transport, providing important guidance for understanding confinement effects and establishing a robust theoretical basis for the regulation of thermal transport.

The impact of Si3N4 incorporation on the mechanical characteristics of ZrB2-SiC nanocomposite sintered via pressureless method.

Due to their unique properties, ultra-high-temperature ceramics possess have great potential for aerospace and industrial applications. In this study, we utilized ZrB2 and Si3N4 powders in micron scale, along with SiC powder in both nano and micron scale. A nanocomposite comprising ZrB2-20 vol% SiC (15 % nano - 5 % micron)-10 % ZrC was incorporated into the base composition by adding Si3N4 in volumes of 1-2-3 volume and 4 %. The process is carried out by pressure-less sintering at 2150 °C. The evaluation in this study involved X-ray diffraction (XRD) analysis, hardness measurement, density determination, fracture toughness assessment, and bending test. The results showed that addition of Si3N4 enhances the relative density, hardness, and fracture toughness of this nanocomposite. The sample with Si3N4volume fraction of 3 % has the best performance, with a relative density of 99.4 %, a hardness of 20.33 GPa, and a fracture toughness of 3.12 MPa M1/2.

Preparation of 3D printed silicon nitride bioceramics by microwave sintering.

Silicon nitride (Si3N4) is a bioceramic material with potential applications. Customization and high reliability are the foundation for the widespread application of Si3N4 bioceramics. This study constructed a new microwave heating structure and successfully prepared 3D printed dense Si3N4 materials, overcoming the adverse effects of a large amount of 3D printed organic forming agents on degreasing and sintering processes, further improving the comprehensive performance of Si3N4 materials. Compared with control materials, the 3D printed Si3N4 materials by microwave sintering have the best mechanical performance: bending strength is 928 MPa, fracture toughness is 9.61 MPa·m1/2. Meanwhile, it has the best biocompatibility and antibacterial properties, and cells exhibit the best activity on the material surface. Research has shown that the excellent mechanical performance and biological activity of materials are mainly related to the high-quality degreasing, high cleanliness sintering environment, and high-quality liquid-phase sintering of materials in microwave environments.

Enhancing Si3N4 Selectivity over SiO2 in Low-RF Power NF3-O2 Reactive Ion Etching: The Effect of NO Surface Reaction.

Highly selective etching of silicon nitride (Si3N4) and silicon dioxide (SiO2) has received considerable attention from the semiconductor community owing to its precise patterning and cost efficiency. We investigated the etching selectivity of Si3N4 and SiO2 in an NF3/O2 radio-frequency glow discharge. The etch rate linearly depended on the source and bias powers, whereas the etch selectivity was affected by the power and ratio of the gas mixture. We found that the selectivity can be controlled by lowering the power with a suitable gas ratio, which affects the surface reaction during the etching process. X-ray photoelectron spectroscopy of the Si3N4 and QMS measurements support the effect of surface reaction on the selectivity change by surface oxidation and nitrogen reduction with the increasing flow of O2. We suggest that the creation of SiOxNy bonds on the surface by NO oxidation is the key mechanism to change the etch selectivity of Si3N4 over SiO2.

Investigation of the Effectiveness of Silicon Nitride as a Reinforcement Agent for Polyethylene Terephthalate Glycol in Material Extrusion 3D Printing.

Polyethylene terephthalate glycol (PETG) and silicon nitride (Si3N4) were combined to create five composite materials with Si3N4 loadings ranging from 2.0 wt.% to 10.0 wt.%. The goal was to improve the mechanical properties of PETG in material extrusion (MEX) additive manufacturing (AM) and assess the effectiveness of Si3N4 as a reinforcing agent for this particular polymer. The process began with the production of filaments, which were subsequently fed into a 3D printer to create various specimens. The specimens were manufactured according to international standards to ensure their suitability for various tests. The thermal, rheological, mechanical, electrical, and morphological properties of the prepared samples were evaluated. The mechanical performance investigations performed included tensile, flexural, Charpy impact, and microhardness tests. Scanning electron microscopy and energy-dispersive X-ray spectroscopy mapping were performed to investigate the structures and morphologies of the samples, respectively. Among all the composites tested, the PETG/6.0 wt.% Si3N4 showed the greatest improvement in mechanical properties (with a 24.5% increase in tensile strength compared to unfilled PETG polymer), indicating its potential for use in MEX 3D printing when enhanced mechanical performance is required from the PETG polymer.

Parallel Grooved Microstructure Manufacturing on the Surface of Si3N4 Ceramics by Femtosecond Laser.

Machining special microstructures on the surface of silicon nitride ceramics helps improve their service performance. However, the high brittleness and low fracture toughness of silicon nitride ceramics make it extremely difficult to machine microstructures on their surface. In this study, a femtosecond laser is used to machine parallel grooved microstructures on the surface of silicon nitride ceramics. The effects of the laser polarization angle, laser single pulse energy, scanning line spacing, and laser scan numbers on the surface morphology and geometric characteristics of grooved microstructures are researched. It is found that a greater angle between the direction of the scanning path and laser polarization is helpful to obtain a smoother surface. As the single pulse energy increases, debris and irregular surface structures will emerge. Increasing the laser scan line spacing leads to clearer and more defined parallel grooved microstructures. The groove depth increases with the increase in the scan numbers. However, when a certain number of scans is reached, the depth will not increase further. This study serves as a valuable research foundation for the femtosecond laser processing of silicon nitride ceramic materials.

Amorphous, Carbonated Calcium Phosphate and Biopolymer-Composite-Coated Si3N4/MWCNTs as Potential Novel Implant Materials.

A biodegradable amorphous carbonated calcium phosphate (caCP)-incorporated polycaprolactone (PCL) composite layer was successfully deposited by a spin coater. In this specific coating, the PCL acts as a bioadhesive, since it provides a better adherence of the coatings to the substrate compared to powder coatings. The caCP-PCL coatings were deposited and formed thin layers on the surface of a Si3N4-3 wt% MWCNT (multiwalled carbon nanotube) substrate, which is an emerging type of implant material in the biomedical field. The composite coatings were examined regarding their morphology, structure and biological performance. The biocompatibility of the samples was tested in vitro with MC3T3-E1 preosteoblast cells. Owing to the caCP-PCL thin layer, the cell viability values were considerably increased compared to the substrate material. The ALP and LDH tests showed numerous living cells on the investrigated coatings. The morphology of the MC3T3-E1 cells was examined by fluorescent staining (calcein and DAPI) and scanning electron microscopy, both of which revealed a well-spread, adhered and confluent monolayer of cells. All performed biocompatibility tests were positive and indicated the applicability of the deposited thin composite layers as possible candidates for orthopaedic implants for an extended period.

The Ablation Performance of Silicon Nitride/Boron Nitride Fibrous Monolithic Ceramics under an Oxyacetylene Combustion Torch.

In this study, Si3N4/BN fibrous monolithic ceramics were successfully prepared by wet spinning extrusion and hot pressing, and the effects on its ablation performance and microstructure were studied. The samples were burned in an oxyacetylene flame for 60 s × 30 to evaluate the ablation resistance. With the increase in ablation time, the fibrous monolithic ceramics exhibited specific mass and linear ablation rates, which show a trend of first increasing, then decreasing, and then increasing again. When the ablation time is 60 s × 10, 60 s × 20, and 60 s × 30, the mass ablation rates of the fibrous monolithic ceramics are 1 × 10-5 mg/s, -8.3 × 10-6 mg/s, -6.7 × 10-7 mg/s, respectively; the linear ablation rates are 4.7 × 10-5 µg/s, -1.2 × 10-5 µg/s and 1.7 × 10-6 µg/s. After 60 s × 30 of ablation, the surface oxides of the species are washed away by the oxyacetylene flame, revealing a porous coral-like structure with many cracks. A glass phase layer, predominantly constituted by sintering aids, envelops the Si3N4 ceramic surface on the ablated sample, serving as an effective barrier against additional ablation.

Thermal Shock Behavior of Si3N4/BN Fibrous Monolithic Ceramics.

To develop materials suitable for aerospace applications, silicon nitride/boron nitride (Si3N4/BN) fibrous monolithic ceramics with varying BN contents were prepared. Employing analytical techniques such as XRD and SEM, coupled with mechanical testing equipment, the influence of BN concentration on the thermal shock resistance of Si3N4/BN fibrous monolithic ceramics was assessed. When the thermal shock differential is less than 800 °C, its residual flexural strength gradually decreases as the thermal shock differential increases. Conversely, when the differential exceeds 1000 °C, the residual flexural strength of the material increases. The residual strength of all samples reached its peak after undergoing a thermal shock assessment at a 1500 °C differential. When the BN mass fraction is 5 wt.%, the residual strength after a thermal shock at a temperature difference of 1500 °C is 387 ± 19 MPa, which is 124% higher than the original strength of the sample that did not undergo thermal shock (25 °C, 311 ± 18 MPa). The oxide layer formed on the thermal shock surface played a role in bridging defects introduced during material surface processing.

Advanced Fabrication Method and Mechanical Properties of Silicon Nitride/Boron Nitride Fibrous Monolithic Ceramics.

Silicon nitride ceramics are regarded as a promising material for high-temperature structural applications due to their remarkable characteristics, including high strength, hardness, thermal conductivity, low dielectric properties, and resistance to creep at elevated temperatures. However, their susceptibility to catastrophic fracture at high temperatures remains a concern. Herein, Si3N4/BN fibrous monolithic ceramics have been successfully prepared by employing wet-spinning and hot-pressing techniques. We delved into the design and optimization of the spinning slurry and examined how the Si3N4/BN fiber diameter affects the ceramics' microstructure and mechanical properties. The spinning slurry exhibited exceptional stability and spinnability. Decreasing the fiber diameter contributed to material densification and improved mechanical properties. Notably, when the fiber diameter is 0.9 mm, the fabricated Si3N4/BN fibrous monolithic ceramics demonstrate a carbon content of 0.82%, a three-point bending strength of 357 ± 24 MPa, and a fracture toughness of 8.8 ± 0.36 MPa·m1/2. This investigation offers valuable insights into producing high-performance Si3N4/BN composite ceramics utilizing hot-pressing technology.

Design of Superlubricity System Using Si3N4/Polyimide as the Friction Pair and Nematic Liquid Crystals as the Lubricant.

Polyimide (PI) is a high-performance engineering plastic used as a bearing material. A superlubricity system using Si3N4/PI as the friction pair and nematic liquid crystals (LCs) as the lubricant was designed. The superlubricity performance was studied by simulating the start-stop condition of the machine, and it was found that the superlubricity system had good reproducibility and stability. In the superlubricity system, friction aligned with the PI molecules, and this alignment was less relevant compared to which substance was rubbing on the PI. Oriented PI molecules induced LC molecule alignment when the pretilt angle was very small, and the LC molecules were almost parallel to the PI molecules due to the one-dimensional ordered arrangement of LC molecules and low viscosity, which is conducive to the occurrence of the superlubricity phenomenon.

Advances in Electrical Discharge Machining of Insulating Ceramics.

There are two main ways of carrying out the electrical discharge machining of the insulating ceramics: changing the electrical and chemical properties of ceramics due to additives in producing composites/nanocomposites and changing the electrical and chemical properties in the interelectrode gap. This review summarizes and analyzes the current data on the machinability in water suspension and hydrocarbons depending on the electrical properties of the ceramic composites and assisting means such as coating and powder. There are provided the existing approaches and original methods for solving the global problem of the electrical discharge machining of insulating ceramics, suggesting further development of the existing methods since, up to now, the experimental research is non-systemic. The dependencies of the machinability on the electrical properties of conductive ceramic composites, the specific electrical resistance of the assisting coating, and the assisting powder's band gap and concentration for machining insulating ceramics are revealed. The higher the electrical conductivity, the higher the machinability of ceramic composites, and the lower the band gap, the higher the machinability for insulating ceramics. Two technological gaps were revealed in the powder's concentration that can be a particular case of logarithmic decrement of attenuation. The proposed approach suggests using assisting powder with the lower band gap.

The shield-like nano-sized Si3N4 derivatives to defend against the attack of lithium dendrites.

The unrestrained Li dendrite growth impedes the performance of Li metal batteries (LMBs) and brings safety concerns. To mitigate the unfavorable effect of Li dendrites, in this work, a shield-like artificial interlayer composed of Si3N4 is employed to achieve the desirable electrochemical performance of LMBs. The Si3N4-based interlayer can in-situ electrochemically react with Li to generate inorganic Li3N and LixSi alloys: the former with high ionic conductivity can effectively enhance the Li+ transference, while the latter with reversibility for Li+ insertion/deinsertion can act as Li+ reservoir to modulate Li+ platting/stripping. Thus, the Si3N4-derived compound shield effectively defends against the attack of Li dendrites and suppresses their growth, with which the Li||Li cells can cycle at 1 mA cm-2 (1 mAh cm-2) up to 500 h and the LiFePO4 (LFP) ||Li batteries can operate 400 cycles at 1C with 91.5 % capacity retention.

Controllable Fabrication and Rectification of Bipolar Nanofluid Diodes in Funnel-Shaped Si3 N4 Nanopores.

Solid-state nanopores attract widespread interest, owning to outstanding robustness, extensive material availability, as well as capability for flexible manufacturing. Bioinspired solid-state nanopores further emerge as potential nanofluidic diodes for mimicking the rectification progress of unidirectional ionic transport in biological K+ channels. However, challenges that remain in rectification are over-reliance on complicated surface modifications and limited control accuracy in size and morphology. In this study, suspended Si3 N4 films of only 100 nm thickness are used as substrate and funnel-shaped nanopores are controllably etched on that with single-nanometer precision, by focused ion beam (FIB) equipped with a flexibly programmable ion dose at any position. A small diameter 7 nm nanopore can be accurately and efficiently fabricated in only 20 ms and verified by a self-designed mathematical model. Without additional modification, funnel-shaped Si3 N4 nanopores functioned as bipolar nanofluidic diodes achieve high rectification by simply filling each side with acidic and basic solution, respectively. Main factors are finely tuned experimentally and simulatively to enhance the controllability. Moreover, nanopore arrays are efficiently prepared to further improve rectification performance, which has great potential for high-throughput practical applications such as extended release of drugs, nanofluidic logic systems, and sensing for environmental monitoring and clinical diagnosis.

Effects of ß-Si3N4 Seeds on Microstructure and Performance of Si3N4 Ceramics in Semiconductor Package.

Among the various ceramic substrate materials, Si3N4 ceramics have demonstrated high thermal conductivity, good thermal shock resistance, and excellent corrosion resistance. As a result, they are well-suited for semiconductor substrates in high-power and harsh conditions encountered in automobiles, high-speed rail, aerospace, and wind power. In this work, Si3N4 ceramics with various ratios of α-Si3N4 and ß-Si3N4 in raw powder form were prepared by spark plasma sintering (SPS) at 1650 °C for 30 min under 30 MPa. When the content of ß-Si3N4 was lower than 20%, with the increase in ß-Si3N4 content, the ceramic grain size changed gradually from 1.5 µm to 1 µm and finally resulted in 2 µm mixed grains. However, As the content of ß-Si3N4 seed crystal increased from 20% to 50%, with the increase in ß-Si3N4 content, the ceramic grain size changed gradually from 1 µm and 2 µm to 1.5 µm. Therefore, when the content of ß-Si3N4 in the raw powder is 20%, the sintered ceramics exhibited a double-peak structure distribution and the best overall performance with a density of 97.5%, fracture toughness of 12.1 MPa·m1/2, and a Vickers hardness of 14.5 GPa. The results of this study are expected to provide a new way of studying the fracture toughness of silicon nitride ceramic substrates.

Optimizing the Rheological and Thermomechanical Response of Acrylonitrile Butadiene Styrene/Silicon Nitride Nanocomposites in Material Extrusion Additive Manufacturing.

The current research aimed to examine the thermomechanical properties of new nanocomposites in additive manufacturing (AM). Material extrusion (MEX) 3D printing was utilized to evolve acrylonitrile butadiene styrene (ABS) nanocomposites with silicon nitride nano-inclusions. Regarding the mechanical and thermal response, the fabricated 3D-printed samples were subjected to a course of standard tests, in view to evaluate the influence of the Si3N4 nanofiller content in the polymer matrix. The morphology and fractography of the fabricated filaments and samples were examined using scanning electron microscopy and atomic force microscopy. Moreover, Raman and energy dispersive spectroscopy tests were accomplished to evaluate the composition of the matrix polymer and nanomaterials. Silicon nitride nanoparticles were proved to induce a significant mechanical reinforcement in comparison with the polymer matrix without any additives or fillers. The optimal mechanical response was depicted to the grade ABS/Si3N4 4 wt. %. An impressive increase in flexural strength (30.3%) and flexural toughness (47.2%) was found. The results validate that these novel ABS nanocomposites with improved mechanical properties can be promising materials.

Study on Tungsten Metallization and Interfacial Bonding of Silicon Nitride High-Temperature Co-Fired Ceramic Substrates.

For the first time, Si3N4 HTCC has been prepared using W as the metal phase by high-temperature co-firing (1830 °C/600 KPa/2 h) as a potential substrate candidate in electronic applications. It was discovered that the addition of Si3N4 to the W paste has a significant impact on thermal expansion coefficient matching and dissolution wetting. As the Si3N4 content increased from 0 to 27.23 vol%, the adhesion strength of W increased continuously from 2.83 kgf/mm2 to 7.04 kgf/mm2. The interfacial bonding of the Si3N4 ceramic and the conduction layer was discussed. SEM analysis confirmed that the interface between Si3N4 and W exhibited an interlocking structure. TEM, HRTEM and XRD indicated the formation of W2C and W5Si3 due to the interface reactions of W with residual carbon and Si3N4, respectively, which contributed to the reactive wetting and good adhesion strength between the interface. Suitable amounts of Si3N4 powder and great interfacial bonding were the main reasons for the tough interfacial matching between the Si3N4 ceramic and the conduction layer.

Mechanisms of the Device Property Alteration Generated by the Proton Irradiation in GaN-Based MIS-HEMTs Using Extremely Thin Gate Insulator.

Recently, we reported that device performance degradation mechanisms, which are generated by the γ-ray irradiation in GaN-based metal-insulator-semiconductor high electron mobility transistors (MIS-HEMTs), use extremely thin gate insulators. When the γ-ray was radiated, the total ionizing dose (TID) effects were generated and the device performance deteriorated. In this work, we investigated the device property alteration and its mechanisms, which were caused by the proton irradiation in GaN-based MIS-HEMTs for the 5 nm-thick Si3N4 and HfO2 gate insulator. The device property, such as threshold voltage, drain current, and transconductance varied by the proton irradiation. When the 5 nm-thick HfO2 layer was employed for the gate insulator, the threshold voltage shift was larger than that of the 5 nm-thick Si3N4 gate insulator, despite the HfO2 gate insulator exhibiting better radiation resistance compared to the Si3N4 gate insulator. On the other hand, the drain current and transconductance degradation were less for the 5 nm-thick HfO2 gate insulator. Unlike the γ-ray irradiation, our systematic research included pulse-mode stress measurements and carrier mobility extraction and revealed that the TID and displacement damage (DD) effects were simultaneously generated by the proton irradiation in GaN-based MIS-HEMTs. The degree of the device property alteration was determined by the competition or superposition of the TID and DD effects for the threshold voltage shift and drain current and transconductance deterioration, respectively. The device property alteration was diminished due to the reduction of the linear energy transfer with increasing irradiated proton energy. We also studied the frequency performance degradation that corresponded to the irradiated proton energy in GaN-based MIS-HEMTs using an extremely thin gate insulator.