The effects of particle size,gradation and solid loading of silicon nitride (Si_(3)N_(4)) on the rheological behavior and curing properties of ceramic slurry are studied by stereolithography (SLA).The results show tha...The effects of particle size,gradation and solid loading of silicon nitride (Si_(3)N_(4)) on the rheological behavior and curing properties of ceramic slurry are studied by stereolithography (SLA).The results show that the particle size of Si_(3)N_(4) powder has a signif icant influence on the rheological properties and stability of the slurry.When m_(D50=1.3μm):m_(D50=2.3μm)=3:7,the slurry viscosity is low and the sedimentation is slow.The most important thing is that with the increase of the solid loading of the slurry,the viscosity of the slurry increases,the stability becomes higher,and the curing thickness decreases.The curing thickness of Si_(3)N_(4) ceramic slurry with solid loading of 50 vol% can reach nearly 50μm.The above results finally show that the process optimizes the formulation of the slurry in rheological and curing properties.展开更多
Silicon nitride (Si 3N 4) has been the main material for balls in ceramic ball bearings, for its lower density, high strength, high hardness, fine thermal stability and anticorrosive, and is widely used in various fie...Silicon nitride (Si 3N 4) has been the main material for balls in ceramic ball bearings, for its lower density, high strength, high hardness, fine thermal stability and anticorrosive, and is widely used in various fields, such as high speed and high temperature areojet engines, precision machine tools and chemical engineer machines. Silicon nitride ceramics is a kind of brittle and hard material that is difficult to machining. In the traditional finishing process of silicon nitride balls, balls are lapped by expensive diamond abrasive. The machining is inefficiency and the cost is high, but also lots of pits, scratch subsurface micro crazes and dislocations will be caused on the surface of the balls, the performance of the ball bearings would be declined seriously. In these year, a kind of new technology known as chemical mechanical polishing is introduced in the ultraprecision machining process of ceramic balls. In this technology, abrasives such as ZrO 2, CeO 2 whose hardness is close to or lower than the work material (Si 3N 4) are used to polishing the balls. In special slurry, these abrasives can chemo-mechanically react with the work material and environment (air or water) to generate softer material (SiO 2). And the resultants will be removed easily at 0.1 nm level. So the surface defects can be minimized, very smooth surface (Ra=4 nm) and fine sphericity (0.15～0.25 μm ) can be obtained, and the machining efficiency is also improved. The action mechanism of the abrasives in the chemical mechanical polishing process in finishing of silicon nitride ball will be introduced in this paper.展开更多
Mechanical properties and corrosion resistance of Si3N4 films are studied by using different experiment parameters, such as plasma enhanced chemical vapor deposition(PECVD) RF power, ratio of reaction gas, reaction pr...Mechanical properties and corrosion resistance of Si3N4 films are studied by using different experiment parameters, such as plasma enhanced chemical vapor deposition(PECVD) RF power, ratio of reaction gas, reaction pressure and working temperature. The etching process of Si3N4 is studied by inductively coupled plasma (ICP) with a gas mixture of SF6 and O2. The influence of the technique parameters, such as ICP power, DC bias, gas composition, total flow rate, on the etching selectivity of Si3N4/EPG533 which is used as a mask layer and the etching rate of Si3N4 is studied, in order to get a better etching selectivity of Si3N4/EPG533 with a faster etching rate of Si3N4. The optimized process parameters of etching Si3N4 by ICP are obtained after a series of experiments and analysis. Under the conditions of total ICP power of 250 W, DC bias of 50W, total flow rate of 40 sccm and O2 composition of 30%, the etching selectivity of 2.05 can be reached when Si3N4 etching rate is 336 nm/min.展开更多
Polyimide(PI)composite films were synthesized incorporating amino modified silicon nitride(Si_(3)N_(4))nanoparticles into PI matrix via in situ polymerization technique.The mechanical and thermal performances as well ...Polyimide(PI)composite films were synthesized incorporating amino modified silicon nitride(Si_(3)N_(4))nanoparticles into PI matrix via in situ polymerization technique.The mechanical and thermal performances as well as the hydrophobic properties of the as prepared composite films were investigated with respect to the dosage of the filler in the PI matrix.According to Thermogravimetric(TGA)analysis,meaningful improvements were achieved in T5(5%weight loss temperature)and T10(10%weight loss temperature)up to 54.1℃ and 52.4℃,respectively when amino functionalized nano Si_(3)N_(4) particles were introduced into the PI matrix.The differential scanning calorimetry(DSC)results revealed that the glass transition temperature(Tg)of the composites was considerably enhanced up to 49.7℃ when amino functionalized Si_(3)N_(4) nanoparticles were incorporated in the PI matrix.Compared to the neat PI,the PI/Si_(3)N_(4) nanocomposites exhibited very high improvement in the tensile strength as well as Young’s modulus up to 105.4%and 138.3%,respectively.Compared to the neat PI,the composites demonstrated highly decreased water absorption behavior which showed about 68.1%enhancement as the content of the nanoparticles was increased to 10 wt%.The SEM(Scanning electron microscope)images confirmed that the enhanced thermal,mechanical and water proof properties are essentially attributed to the improved compatibility of the filler with the matrix and hence,enhanced distribution inside the matrix because of the amino groups on the surface of Si_(3)N_(4) nanoparticles obtained from surface functionalization.展开更多
In this paper,Si3N4 fiber materials were fabricated by nitridation of porous Si green bodies,which were prepared by the foaming method combined with gel-casting.The effect of the nitriding process(the heating rate and...In this paper,Si3N4 fiber materials were fabricated by nitridation of porous Si green bodies,which were prepared by the foaming method combined with gel-casting.The effect of the nitriding process(the heating rate and the nitrogen flow rate)on the phase and the microstructure was studied.The results show that decreasing the heating rate and the nitrogen flow rate is both beneficial to the growth of Si3N4 nanofibers and promoting the disintegration of the pore wall structure of the porous green bodies.The optimized nitrogen flow rate and the heating rate for the growth of silicon nitride fibers are 150 mL/min and 0.5℃/min,respectively.展开更多
Porous Si3N4-SiO2-based ceramics with different porosity were prepared via free sintering of Si3N4 on air with an addition of semolina (5, 10 and 20 wt%) as a pore-forming agent. The semolina content in the starting p...Porous Si3N4-SiO2-based ceramics with different porosity were prepared via free sintering of Si3N4 on air with an addition of semolina (5, 10 and 20 wt%) as a pore-forming agent. The semolina content in the starting powder controlled the volume fraction of pores in the sintered body. Small pores (5 μm) formed a continuous network in the whole volume of the ceramic material, while the large pores (~100 μm), formed from the added semolina were mostly isolated in the ceramic matrix. Mercury porosimetry and strength measurements have shown that specific surface area, volume density and compressive strength decreased with the amount of semolina in the samples. Mechanical properties similar to bone were obtained for the sample with 20 wt% semolina pore forming agent (compressive strength 350 MPa, density 2.17 g.cm-3). The prepared Si3N4-SiO2-based ceramics were evaluated for cytotoxic and genotoxic potential on human fibroblast VH10 and B-HNF-1 cells. Biological tests have shown that both these human fibroblast cell lines were sensitive to the samples with lower porosity and cell growth inhibition was observed in the range 14.9% - 21.3%. The cytotoxicity of the sample with the highest porosity (~40%) was not significant (10%). The microscopic observations have shown that VH10 and B-HNF-1 cells growing around the silicon nitride ceramic discs were homogeneously distributed on the cultivation surface. No significant morphologic changes were found in treated cells, their morphology was very similar to that of the control cells. None of the tested Si3N4-based ceramic samples induced necrotic/apoptotic death of human fibroblasts. Sample S-20 had similar properties to bones and was characterized by very good biocompatibility, slight cytotoxicity and none genotoxicity. Therefore, Si3N4-SiO2-based ceramics prepared by free sintering on air are potential biomaterials for medical applications.展开更多
Amorphous hydrogenated silicon nitride thin films a-SiN<sub>x</sub>:H (abbreviated later by SiN<sub>x</sub>) were deposited by Electron Cyclotron Resonance plasma enhanced chemical vapor deposi...Amorphous hydrogenated silicon nitride thin films a-SiN<sub>x</sub>:H (abbreviated later by SiN<sub>x</sub>) were deposited by Electron Cyclotron Resonance plasma enhanced chemical vapor deposition method (ECR-PECVD). By changing ratio of gas flow (R = NH<sub>3</sub>/SiH<sub>4</sub>) in the reactor chamber different stoichiometric layers x = [N]/[Si] ([N] and [Si] atomic concentrations) are successfully deposited. Part of the obtained films has subsequently undergone rapid thermal annealing RTA (800°C/1 s) using halogen lamps. Optical and structural characterizations are then achieved by spectroscopic ellipsometry (SE), ion beam analysis and infrared absorption techniques. The SE measurements show that the tuning character of their refractive index n(λ) with stoichiometry x and their non-absorption properties in the range of 250 - 850 nm expect for Si-rich SiN<sub>x</sub> films in the ultraviolet UV range. The stoichiometry x and its depth profile are determined by Rutherford backscattering spectrometry (RBS) while the hydrogen profile (atomic concentration) is determined by Elastic Recoil Detection Analysis (ERDA). Vibrational characteristics of the Si-N, Si-H and N-H chemical bonds in the silicon nitride matrix are investigated by infrared absorption. An atomic hydrogen fraction ranging from 12% to 22% uniformly distributed as evaluated by ERDA is depending inversely on the stoichiometry x ranging from 0.34 to 1.46 as evaluated by RBS for the studied SiN<sub>x</sub> films. The hydrogen loss after RTA process and its out-diffusion depend strongly on the chemical structure of the films and less on the initial hydrogen concentration. A large hydrogen loss was noted for non-thermally stable Si-rich SiNx films. Rich nitrogen films are less sensitive to rapid thermal process.展开更多
We designed a reconfigurable dual-interferometer coupled silicon nitride microring resonator.By tuning the integrated heater on interferometer's arms,the"critical coupling"bandwidth of resonant mode is c...We designed a reconfigurable dual-interferometer coupled silicon nitride microring resonator.By tuning the integrated heater on interferometer's arms,the"critical coupling"bandwidth of resonant mode is continuously adjustable whose quality factor varies from 7.9×10^(4) to 1.9×10^(5) with the extinction ratio keeping higher than 25 dB.Also a variety of coupling spanning from"under-coupling"to"over-coupling"were achieved,showing the ability to tune the quality factor from 6.0×10^(3) to 2.3×10^(5).Our design can provide an adjustable filtering method on silicon nitride photonic chip and contribute to optimize the nonlinear process for quantum photonics and all-optical signal processing.展开更多
The influence of the residual stress in surface of ceramic balls on the fatigue life is large, because the life of silicon nitride ball bearings is more sensitive to the load acted on the bearings than the life of all...The influence of the residual stress in surface of ceramic balls on the fatigue life is large, because the life of silicon nitride ball bearings is more sensitive to the load acted on the bearings than the life of all-steel ball bearings. In this paper, the influence of thermal stress produced in sintering and mechanical stress formed in lapping process on residual stress in surface of silicon nitride ceramic balls was discussed. The residual compress stress will be formed in the surface of silicon nitride ceramic balls after sintering. The residual tensile stress will be formed in surface of silicon nitride ceramic balls in lapping process, and the size of abrasive particle is smaller, such trend is stronger. In this paper the residual stress was measured by the xylometric measurement in which the material in surface was peeled with lapping. The distribution of residual stress in surface can be calculated with the variation in specific volume. The technological parameter with which the material was peeled by lapping was given, for minimizing the extra influence of the residual stress forming in peeling on the original residual stress in surface, the abrasive particle size would not be too small and the load impressed would not be too large. Some experimental researches on residual stress in surface of silicon nitride ceramic balls were made. The surface of silicon nitride ceramic balls presented residual compressive stress after sintering and the influence of the ball size on the residual stress is feeble. It is expected that the size of ball blank is same for achieving the same residual compressive stress in surface on balls after final machining. In lapping process, the surface of silicon nitride ceramic balls presented residual tensile stress, the larger the load which is impressed on single ball, the larger the amplitude of residual tensile stress is; the smaller the abrasive particle, the stronger the trend of plastic deformation is and the larger the amplitude of residual tensile stress is.展开更多
Electro-optic modulator is a key component for on-chip optical signal processing.An electro-optic phase modulator based on multilayer graphene embedded in silicon nitride waveguide is demonstrated to fulfill low-power...Electro-optic modulator is a key component for on-chip optical signal processing.An electro-optic phase modulator based on multilayer graphene embedded in silicon nitride waveguide is demonstrated to fulfill low-power operation.Finite element method is adopted to investigate the interaction enhancement between the graphene flake and the optical mode.The impact of multilayer graphene on the performance of phase modulator is studied comprehensively.Simulation results show that the modulation efficiency improves with the increment of graphene layer number,as well as the modulation length.The 3-dB bandwidth of around 48 GHz is independent of graphene layer number and length.Compared to modulator with two-or four-layer graphene,the six-layer graphene/silicon nitride waveguide modulator can realizeπphase shift at a low-power consumption of 14 fJ/bit when the modulation length is 240μm.展开更多
Silicon nitride(Si_(3)N_(4))supported cobalt catalysts(Co/Si_(3)N_(4))were fabricated by using wetness impregnation procedure.The microscopic morphology,phase composition,and electronic states were characterized by XR...Silicon nitride(Si_(3)N_(4))supported cobalt catalysts(Co/Si_(3)N_(4))were fabricated by using wetness impregnation procedure.The microscopic morphology,phase composition,and electronic states were characterized by XRD,TEM,SEM,and XPS,respectively.For comparison,cobalt catalyst supported on SiO_(2)(Co/SiO_(2))was also investigated.XPS studies and DFT calculations show that the cobalt species in Co/Si_(3)N_(4) have lower valence state than those in Co/SiO_(2).The catalytic ESR reactions demonstrate that Co/Si_(3)N_(4) exhibits distinctly higher catalytic activity and hydrogen selectivity than Si_(3)N_(4) support and Co/SiO_(2) catalyst with the identical cobalt loading,indicative of the favorable effect of Si_(3)N_(4) support on the catalytic performance of supported cobalt catalyst.Durability tests and TG-DSC studies show that Co/Si_(3)N_(4) catalyst exhibits better stability and resistance to coke during the same catalytic experiment period.展开更多
The inductively coupled plasma chemical vapor deposition(ICP-CVD) deposited silicon nitride(SiN_(x)) thin film was evaluated for its application as the electrical insulating film for a capacitor device.In order to ach...The inductively coupled plasma chemical vapor deposition(ICP-CVD) deposited silicon nitride(SiN_(x)) thin film was evaluated for its application as the electrical insulating film for a capacitor device.In order to achieve highest possible dielectric strength of SiN_(x),the process parameters of ICP-CVD were carefully tuned to control hydrogen in SiN_(x) films by means of tuning N_(2)/SiH_(4) ratio and radio frequency(RF) power.Besides electrical measurements,the hydrogen content in the films was measured by dynamic secondary ion mass spectrometry(D-SIMS).Fourier transform infrared spectroscopy(FTIR) and micro Raman spectroscopy were used to characterize the SiN_(x) films by measuring Si-H and N-H bonds’ intensities.It was found that the more Si-H bonds lead to the higher dielectric strength.展开更多
Hydrogenated amorphous silicon nitride (a-SiN<sub>x</sub>:H) films have been grown from a SiH<sub>4</sub>–N<sub>2</sub> gas mixture through very high frequency (VHF) plasma-enhance...Hydrogenated amorphous silicon nitride (a-SiN<sub>x</sub>:H) films have been grown from a SiH<sub>4</sub>–N<sub>2</sub> gas mixture through very high frequency (VHF) plasma-enhanced chemical vapor deposition (PECVD) at 50℃. The films are dense and transparent in the visible region. The peak frequency of the Si–N stretching mode in the IR absorption spectrum increases with increasing N–H bond density, which is similar to the behavior of a-SiN<sub>x</sub>:H films grown from SiH<sub>4</sub>–NH<sub>3</sub> gas. During storage in a dry air atmosphere, the Si–O absorption increases. A large shift in the peak frequency of the Si–N stretching mode in the initial stage of oxidation, which is higher than the shift expected from the increase in the N–H bond density, is mainly caused by the change in the sum of electronegativity of nearest neighbors around the Si–N bond due to the increase in the Si–O bond density.展开更多
High-thermal-conductivity silicon nitride ceramic substrates are indispensable components for nextgeneration high-power electronic devices because of their excellent mechanical properties and high thermal conductiviti...High-thermal-conductivity silicon nitride ceramic substrates are indispensable components for nextgeneration high-power electronic devices because of their excellent mechanical properties and high thermal conductivities, which make them suitable for applications in complex and extreme environments. Here, we present an overview of the recent developments in the preparation of high-thermal-conductivity silicon nitride ceramics. First,the factors affecting the thermal conductivity of silicon nitride ceramics are described. These include lattice oxygen and grain boundary phases, as well the oxygen content of the crystal lattice, which is the main influencing factor.Then, the methods to prepare high-thermal-conductivity silicon nitride ceramics are presented. Recent work on the preparation of high-thermal-conductivity silicon nitride is described in detail, including the raw materials used and the forming and sintering processes. Although great progress has been made, the development of a high-quality,low-cost fabrication process remains a challenge. Nevertheless, we believe that high-thermal-conductivity silicon nitride substrates are promising for massive practical applications in the next generation of high-power electronic devices.展开更多
The micro-crystalline diamond (MCD) and fine-grained diamond (FGD) films are deposited on commercial silicon nitride inserts by the hot-filament chemical vapor deposition (HFCVD) method. The friction andcutting proper...The micro-crystalline diamond (MCD) and fine-grained diamond (FGD) films are deposited on commercial silicon nitride inserts by the hot-filament chemical vapor deposition (HFCVD) method. The friction andcutting properties of as-deposited MCD and FGD films coated silicon nitride (Si3N4) inserts are comparatively investigated in this study. The scanning electron microscopy (SEM) and Raman spectroscopy are adopted to studythe characterization of the deposited diamond films. The friction tests are conducted on a ball-on-plate typereciprocating friction tester in ambient air using Co-cemented tungsten carbide (WC-Co), Si3N4 and ball-bearing steel (BBS) balls as the mating materials of the diamond films. For sliding against WC-Co, Si3N4 and BBS,the FGD film presents lower friction coeffcients than the MCD film. However, after sliding against Si3N4, the FGD film is subject to more severe wear than the MCD film. The cutting performance of as-deposited MCD and FGD coated Si3N4 inserts is examined in dry turning glass fiber reinforced plastics (GFRP) composite materials,comparing with the uncoated Si3N4 insert. The results indicate that the lifetime of Si3N4 inserts can be prolonged by depositing the MCD or FGD film on them and the FGD coated insert shows longer cutting lifetime than the MCD coated one.展开更多
Kerr frequency combs have been attracting significant interest due to their rich physics and broad applications in metrology,microwave photonics,and telecommunications.In this review,we first introduce the fundamental...Kerr frequency combs have been attracting significant interest due to their rich physics and broad applications in metrology,microwave photonics,and telecommunications.In this review,we first introduce the fundamental physics,master equations,simulation methods,and dynamic process of Kerr frequency combs.We then analyze the most promising material platform for realizing Kerr frequency combs—silicon nitride on insulator(SNOI)in comparison with other material platforms.Moreover,we discuss the fabrication methods,process optimization as well as tuning and measurement schemes of SNOI-based Kerr frequency combs.Furthermore,we highlight several emerging applications of Kerr frequency combs in metrology,including spectroscopy,ranging,and timing.Finally,we summarize this review and envision the future development of chip-scale Kerr frequency combs from the viewpoint of theory,material platforms,and tuning methods.展开更多
The slab effective index difference between the transverse-electric(TE)and transverse-magnetic(TM)polarizations was utilized to obtain complete photonic bandgap(CPBG)in a silicon nitride(Si_(x)N_(y))photonic crystal s...The slab effective index difference between the transverse-electric(TE)and transverse-magnetic(TM)polarizations was utilized to obtain complete photonic bandgap(CPBG)in a silicon nitride(Si_(x)N_(y))photonic crystal slab.For this,coincident frequency range in the TE photonic bandgap(PBG)and TM PBG,which denotes the CPBGs of the slab,must be found with the same structure.Through adjusting the effective index pair of TE and TM polarizations by changing the thickness of the Si_(x)N_(y)core layer,and also optimizing the structure parameters within the photonic crystal plane,a large normalized CPBG of 5.62%was theoretically obtained in a slab of Si_(x)N_(y)with a refractive index of 2.5.Moreover,based on the obtained CPBG,a microcavity which could support both TE and TM polarization was theoretically demonstrated.The cavity modes for different polarizations were both well confined,which proved the reliability of the CPBG.In addition,using the same method,the lowest refractive index of Si_(x)N_(y)on silica slab for a CPBG could be extended to as low as 2.The results indicate that there is potential for development of various high-performance CPBG devices based on Si_(x)N_(y)slab technology.展开更多
Steam oxidation resistance of Si3N4 and Si2N2O as well as SiAlON bonded SiC refractories at 900℃was tested according to ASTM-C863.Phase composition and microstructure before and after oxidation were analyzed by XRD a...Steam oxidation resistance of Si3N4 and Si2N2O as well as SiAlON bonded SiC refractories at 900℃was tested according to ASTM-C863.Phase composition and microstructure before and after oxidation were analyzed by XRD and SEM.The results show that Si3N4 and Si2N2O bonded SiC refractory presents better steam oxidation resistance than SiAlON bonded SiC.For Si3N4 and Si2N2O bonded SiC,the oxidation speed is higher with more pronounced volume expansion in the early 100 h;afterwards,the volume expansion slows down gradually and starts to level off after 300 h.It is considered that the high silica glass phase formed during the oxidation covers Si3N4 and Si2N2O,and SiC as a protective layer and fills the open pores.But for SiAlON bonded SiC,the volume expands gradually and constantly with the increasing oxidation duration even after 500 h,due to the continuous formation of mullite transformed from oxidation products and Al2O3 in SiAlON.展开更多
In order to investigate the effect of the catalyst loading mode on the mechanical properties of Si_(3)N_(4) composite MgO-C refractories prepared by nitridation,fused magnesia,flake graphite,silicon powder,and phenoli...In order to investigate the effect of the catalyst loading mode on the mechanical properties of Si_(3)N_(4) composite MgO-C refractories prepared by nitridation,fused magnesia,flake graphite,silicon powder,and phenolic resin were used as the main raw materials,and ferric nitrate as the catalyst to prepare refractories by nitriding at 1350℃.The effects of different catalyst supports(silicon powder,silicon powder+phenolic resin)on the formation of Si_(3)N_(4) in MgO-C refractories and the properties of refractories were studied.The results show that the silicon powder+resin catalyst support promotes the participation ofα-Si_(3)N_(4) in the reaction to generateβ-Si_(3)N_(4) and MgSiN_(2),and generates more SiC.However,this loading mode causes more gas to escape from the refractories and loosens the material structure,which reduces the mechanical properties.On the contrary,MgO-C refractories prepared by nitridation with silicon powder-supported catalysts under the same conditions show higher density and better mechanical properties.展开更多
Laser assisted machining is an effective method to machine advanced materials with the added benefits of longer tool life and increased material removal rates. While extensive studies have investigated the machining p...Laser assisted machining is an effective method to machine advanced materials with the added benefits of longer tool life and increased material removal rates. While extensive studies have investigated the machining properties for laser assisted milling(LAML),few attempts have been made to extend LAML to machining parts with complex geometric features. A methodology for continuous path machining for LAML is developed by integration of a rotary and movable table into an ordinary milling machine with a laser beam system. The machining strategy and processing path are investigated to determine alignment of the machining path with the laser spot.In order to keep the material removal temperatures above the softening temperature of silicon nitride, the transformation is coordinated and the temperature interpolated, establishing a transient thermal model. The temperatures of the laser center and cutting zone are also carefully controlled to achieve optimal machining results and avoid thermal damage. These experiments indicate that the system results in no surface damage as well as good surface roughness, validating the application of this machining strategy and thermal model in the development of a new LAML system for continuous path processing of silicon nitride. The proposed approach can be easily applied in LAML system to achieve continuous processing and improve efficiency in laser assisted machining.展开更多
基金Funded by National Natural Science Foundation of China (No.43200021)。
文摘The effects of particle size,gradation and solid loading of silicon nitride (Si_(3)N_(4)) on the rheological behavior and curing properties of ceramic slurry are studied by stereolithography (SLA).The results show that the particle size of Si_(3)N_(4) powder has a signif icant influence on the rheological properties and stability of the slurry.When m_(D50=1.3μm):m_(D50=2.3μm)=3:7,the slurry viscosity is low and the sedimentation is slow.The most important thing is that with the increase of the solid loading of the slurry,the viscosity of the slurry increases,the stability becomes higher,and the curing thickness decreases.The curing thickness of Si_(3)N_(4) ceramic slurry with solid loading of 50 vol% can reach nearly 50μm.The above results finally show that the process optimizes the formulation of the slurry in rheological and curing properties.
文摘Silicon nitride (Si 3N 4) has been the main material for balls in ceramic ball bearings, for its lower density, high strength, high hardness, fine thermal stability and anticorrosive, and is widely used in various fields, such as high speed and high temperature areojet engines, precision machine tools and chemical engineer machines. Silicon nitride ceramics is a kind of brittle and hard material that is difficult to machining. In the traditional finishing process of silicon nitride balls, balls are lapped by expensive diamond abrasive. The machining is inefficiency and the cost is high, but also lots of pits, scratch subsurface micro crazes and dislocations will be caused on the surface of the balls, the performance of the ball bearings would be declined seriously. In these year, a kind of new technology known as chemical mechanical polishing is introduced in the ultraprecision machining process of ceramic balls. In this technology, abrasives such as ZrO 2, CeO 2 whose hardness is close to or lower than the work material (Si 3N 4) are used to polishing the balls. In special slurry, these abrasives can chemo-mechanically react with the work material and environment (air or water) to generate softer material (SiO 2). And the resultants will be removed easily at 0.1 nm level. So the surface defects can be minimized, very smooth surface (Ra=4 nm) and fine sphericity (0.15～0.25 μm ) can be obtained, and the machining efficiency is also improved. The action mechanism of the abrasives in the chemical mechanical polishing process in finishing of silicon nitride ball will be introduced in this paper.
文摘Mechanical properties and corrosion resistance of Si3N4 films are studied by using different experiment parameters, such as plasma enhanced chemical vapor deposition(PECVD) RF power, ratio of reaction gas, reaction pressure and working temperature. The etching process of Si3N4 is studied by inductively coupled plasma (ICP) with a gas mixture of SF6 and O2. The influence of the technique parameters, such as ICP power, DC bias, gas composition, total flow rate, on the etching selectivity of Si3N4/EPG533 which is used as a mask layer and the etching rate of Si3N4 is studied, in order to get a better etching selectivity of Si3N4/EPG533 with a faster etching rate of Si3N4. The optimized process parameters of etching Si3N4 by ICP are obtained after a series of experiments and analysis. Under the conditions of total ICP power of 250 W, DC bias of 50W, total flow rate of 40 sccm and O2 composition of 30%, the etching selectivity of 2.05 can be reached when Si3N4 etching rate is 336 nm/min.
基金the National Natural Science Foundation of China(51373044)Natural Science Foundation of Heilongjiang Province of China(E2017018).
文摘Polyimide(PI)composite films were synthesized incorporating amino modified silicon nitride(Si_(3)N_(4))nanoparticles into PI matrix via in situ polymerization technique.The mechanical and thermal performances as well as the hydrophobic properties of the as prepared composite films were investigated with respect to the dosage of the filler in the PI matrix.According to Thermogravimetric(TGA)analysis,meaningful improvements were achieved in T5(5%weight loss temperature)and T10(10%weight loss temperature)up to 54.1℃ and 52.4℃,respectively when amino functionalized nano Si_(3)N_(4) particles were introduced into the PI matrix.The differential scanning calorimetry(DSC)results revealed that the glass transition temperature(Tg)of the composites was considerably enhanced up to 49.7℃ when amino functionalized Si_(3)N_(4) nanoparticles were incorporated in the PI matrix.Compared to the neat PI,the PI/Si_(3)N_(4) nanocomposites exhibited very high improvement in the tensile strength as well as Young’s modulus up to 105.4%and 138.3%,respectively.Compared to the neat PI,the composites demonstrated highly decreased water absorption behavior which showed about 68.1%enhancement as the content of the nanoparticles was increased to 10 wt%.The SEM(Scanning electron microscope)images confirmed that the enhanced thermal,mechanical and water proof properties are essentially attributed to the improved compatibility of the filler with the matrix and hence,enhanced distribution inside the matrix because of the amino groups on the surface of Si_(3)N_(4) nanoparticles obtained from surface functionalization.
基金This work was supported by the National Natural Science Foundation of China(NSFC-No.51672256)National Natural Science Foundation of China-Key Projects of Henan United Fund(NSFC-No.U1904217).
文摘In this paper,Si3N4 fiber materials were fabricated by nitridation of porous Si green bodies,which were prepared by the foaming method combined with gel-casting.The effect of the nitriding process(the heating rate and the nitrogen flow rate)on the phase and the microstructure was studied.The results show that decreasing the heating rate and the nitrogen flow rate is both beneficial to the growth of Si3N4 nanofibers and promoting the disintegration of the pore wall structure of the porous green bodies.The optimized nitrogen flow rate and the heating rate for the growth of silicon nitride fibers are 150 mL/min and 0.5℃/min,respectively.
基金This study was supported by the Technology Assistance Agency under the contract no.APVV-0500-10the Slovak State Committee for Scientific Research VEGA,grant 1/0165/10.
文摘Porous Si3N4-SiO2-based ceramics with different porosity were prepared via free sintering of Si3N4 on air with an addition of semolina (5, 10 and 20 wt%) as a pore-forming agent. The semolina content in the starting powder controlled the volume fraction of pores in the sintered body. Small pores (5 μm) formed a continuous network in the whole volume of the ceramic material, while the large pores (~100 μm), formed from the added semolina were mostly isolated in the ceramic matrix. Mercury porosimetry and strength measurements have shown that specific surface area, volume density and compressive strength decreased with the amount of semolina in the samples. Mechanical properties similar to bone were obtained for the sample with 20 wt% semolina pore forming agent (compressive strength 350 MPa, density 2.17 g.cm-3). The prepared Si3N4-SiO2-based ceramics were evaluated for cytotoxic and genotoxic potential on human fibroblast VH10 and B-HNF-1 cells. Biological tests have shown that both these human fibroblast cell lines were sensitive to the samples with lower porosity and cell growth inhibition was observed in the range 14.9% - 21.3%. The cytotoxicity of the sample with the highest porosity (~40%) was not significant (10%). The microscopic observations have shown that VH10 and B-HNF-1 cells growing around the silicon nitride ceramic discs were homogeneously distributed on the cultivation surface. No significant morphologic changes were found in treated cells, their morphology was very similar to that of the control cells. None of the tested Si3N4-based ceramic samples induced necrotic/apoptotic death of human fibroblasts. Sample S-20 had similar properties to bones and was characterized by very good biocompatibility, slight cytotoxicity and none genotoxicity. Therefore, Si3N4-SiO2-based ceramics prepared by free sintering on air are potential biomaterials for medical applications.
文摘Amorphous hydrogenated silicon nitride thin films a-SiN<sub>x</sub>:H (abbreviated later by SiN<sub>x</sub>) were deposited by Electron Cyclotron Resonance plasma enhanced chemical vapor deposition method (ECR-PECVD). By changing ratio of gas flow (R = NH<sub>3</sub>/SiH<sub>4</sub>) in the reactor chamber different stoichiometric layers x = [N]/[Si] ([N] and [Si] atomic concentrations) are successfully deposited. Part of the obtained films has subsequently undergone rapid thermal annealing RTA (800°C/1 s) using halogen lamps. Optical and structural characterizations are then achieved by spectroscopic ellipsometry (SE), ion beam analysis and infrared absorption techniques. The SE measurements show that the tuning character of their refractive index n(λ) with stoichiometry x and their non-absorption properties in the range of 250 - 850 nm expect for Si-rich SiN<sub>x</sub> films in the ultraviolet UV range. The stoichiometry x and its depth profile are determined by Rutherford backscattering spectrometry (RBS) while the hydrogen profile (atomic concentration) is determined by Elastic Recoil Detection Analysis (ERDA). Vibrational characteristics of the Si-N, Si-H and N-H chemical bonds in the silicon nitride matrix are investigated by infrared absorption. An atomic hydrogen fraction ranging from 12% to 22% uniformly distributed as evaluated by ERDA is depending inversely on the stoichiometry x ranging from 0.34 to 1.46 as evaluated by RBS for the studied SiN<sub>x</sub> films. The hydrogen loss after RTA process and its out-diffusion depend strongly on the chemical structure of the films and less on the initial hydrogen concentration. A large hydrogen loss was noted for non-thermally stable Si-rich SiNx films. Rich nitrogen films are less sensitive to rapid thermal process.
基金the National Key Research and Development Program of China(Grant Nos.2019YFA0308700and 2017YFA0303700)the National Natural Science Foundation of China(Grant Nos.11627810 and 11690031)the Open Funds from the State Key Laboratory of High Performance Computing of China(HPCL,National University of Defense Technology).
文摘We designed a reconfigurable dual-interferometer coupled silicon nitride microring resonator.By tuning the integrated heater on interferometer's arms,the"critical coupling"bandwidth of resonant mode is continuously adjustable whose quality factor varies from 7.9×10^(4) to 1.9×10^(5) with the extinction ratio keeping higher than 25 dB.Also a variety of coupling spanning from"under-coupling"to"over-coupling"were achieved,showing the ability to tune the quality factor from 6.0×10^(3) to 2.3×10^(5).Our design can provide an adjustable filtering method on silicon nitride photonic chip and contribute to optimize the nonlinear process for quantum photonics and all-optical signal processing.
文摘The influence of the residual stress in surface of ceramic balls on the fatigue life is large, because the life of silicon nitride ball bearings is more sensitive to the load acted on the bearings than the life of all-steel ball bearings. In this paper, the influence of thermal stress produced in sintering and mechanical stress formed in lapping process on residual stress in surface of silicon nitride ceramic balls was discussed. The residual compress stress will be formed in the surface of silicon nitride ceramic balls after sintering. The residual tensile stress will be formed in surface of silicon nitride ceramic balls in lapping process, and the size of abrasive particle is smaller, such trend is stronger. In this paper the residual stress was measured by the xylometric measurement in which the material in surface was peeled with lapping. The distribution of residual stress in surface can be calculated with the variation in specific volume. The technological parameter with which the material was peeled by lapping was given, for minimizing the extra influence of the residual stress forming in peeling on the original residual stress in surface, the abrasive particle size would not be too small and the load impressed would not be too large. Some experimental researches on residual stress in surface of silicon nitride ceramic balls were made. The surface of silicon nitride ceramic balls presented residual compressive stress after sintering and the influence of the ball size on the residual stress is feeble. It is expected that the size of ball blank is same for achieving the same residual compressive stress in surface on balls after final machining. In lapping process, the surface of silicon nitride ceramic balls presented residual tensile stress, the larger the load which is impressed on single ball, the larger the amplitude of residual tensile stress is; the smaller the abrasive particle, the stronger the trend of plastic deformation is and the larger the amplitude of residual tensile stress is.
基金the National Key Research and Development Program of China(Grant No.2019YFB2203001)the National Natural Science Foundation of China(Grant Nos.61675087,61875069,and 61605057)the Science and Technology Development Plan of Jilin Province,China(Grant No.JJKH20190118KJ).
文摘Electro-optic modulator is a key component for on-chip optical signal processing.An electro-optic phase modulator based on multilayer graphene embedded in silicon nitride waveguide is demonstrated to fulfill low-power operation.Finite element method is adopted to investigate the interaction enhancement between the graphene flake and the optical mode.The impact of multilayer graphene on the performance of phase modulator is studied comprehensively.Simulation results show that the modulation efficiency improves with the increment of graphene layer number,as well as the modulation length.The 3-dB bandwidth of around 48 GHz is independent of graphene layer number and length.Compared to modulator with two-or four-layer graphene,the six-layer graphene/silicon nitride waveguide modulator can realizeπphase shift at a low-power consumption of 14 fJ/bit when the modulation length is 240μm.
基金by the National Natural Science Foundation of China(Nos.21671154,U1732147)the Key Laboratory of Hubei Province for Coal Conversion and New Carbon Materials(WKDM202210)the State Key Laboratory of Refractories(SKLAR202009)。
文摘Silicon nitride(Si_(3)N_(4))supported cobalt catalysts(Co/Si_(3)N_(4))were fabricated by using wetness impregnation procedure.The microscopic morphology,phase composition,and electronic states were characterized by XRD,TEM,SEM,and XPS,respectively.For comparison,cobalt catalyst supported on SiO_(2)(Co/SiO_(2))was also investigated.XPS studies and DFT calculations show that the cobalt species in Co/Si_(3)N_(4) have lower valence state than those in Co/SiO_(2).The catalytic ESR reactions demonstrate that Co/Si_(3)N_(4) exhibits distinctly higher catalytic activity and hydrogen selectivity than Si_(3)N_(4) support and Co/SiO_(2) catalyst with the identical cobalt loading,indicative of the favorable effect of Si_(3)N_(4) support on the catalytic performance of supported cobalt catalyst.Durability tests and TG-DSC studies show that Co/Si_(3)N_(4) catalyst exhibits better stability and resistance to coke during the same catalytic experiment period.
基金Project supported by the Natural Science Foundation of Jiangsu Higher Education Institutions of China(Grant Nos.19KJD140002 and 19KJB140008)the Key Projects of Ministry of Science and Technology of China(Grant No.SQ2020YFF0407077)+3 种基金Postgraduate Research&Practice Innovation Program of Jiangsu Province,China(Grant Nos.2020XKT786 and KYCX202337)the National Foreign Experts Bureau High-end Foreign Experts Project,China(Grant No.G20190114003)the Key Research and Development Program of Jiangsu Province,China(Grant No.BE2018063)the Scientific Research Program for Doctoral Teachers of JSNU(Grant No.9212218113)。
文摘The inductively coupled plasma chemical vapor deposition(ICP-CVD) deposited silicon nitride(SiN_(x)) thin film was evaluated for its application as the electrical insulating film for a capacitor device.In order to achieve highest possible dielectric strength of SiN_(x),the process parameters of ICP-CVD were carefully tuned to control hydrogen in SiN_(x) films by means of tuning N_(2)/SiH_(4) ratio and radio frequency(RF) power.Besides electrical measurements,the hydrogen content in the films was measured by dynamic secondary ion mass spectrometry(D-SIMS).Fourier transform infrared spectroscopy(FTIR) and micro Raman spectroscopy were used to characterize the SiN_(x) films by measuring Si-H and N-H bonds’ intensities.It was found that the more Si-H bonds lead to the higher dielectric strength.
文摘Hydrogenated amorphous silicon nitride (a-SiN<sub>x</sub>:H) films have been grown from a SiH<sub>4</sub>–N<sub>2</sub> gas mixture through very high frequency (VHF) plasma-enhanced chemical vapor deposition (PECVD) at 50℃. The films are dense and transparent in the visible region. The peak frequency of the Si–N stretching mode in the IR absorption spectrum increases with increasing N–H bond density, which is similar to the behavior of a-SiN<sub>x</sub>:H films grown from SiH<sub>4</sub>–NH<sub>3</sub> gas. During storage in a dry air atmosphere, the Si–O absorption increases. A large shift in the peak frequency of the Si–N stretching mode in the initial stage of oxidation, which is higher than the shift expected from the increase in the N–H bond density, is mainly caused by the change in the sum of electronegativity of nearest neighbors around the Si–N bond due to the increase in the Si–O bond density.
基金financially supported by the National Key Research and Development Program of China (No.2017YFB0310400)the National Natural Science Foundation of China (No.51427802)。
文摘High-thermal-conductivity silicon nitride ceramic substrates are indispensable components for nextgeneration high-power electronic devices because of their excellent mechanical properties and high thermal conductivities, which make them suitable for applications in complex and extreme environments. Here, we present an overview of the recent developments in the preparation of high-thermal-conductivity silicon nitride ceramics. First,the factors affecting the thermal conductivity of silicon nitride ceramics are described. These include lattice oxygen and grain boundary phases, as well the oxygen content of the crystal lattice, which is the main influencing factor.Then, the methods to prepare high-thermal-conductivity silicon nitride ceramics are presented. Recent work on the preparation of high-thermal-conductivity silicon nitride is described in detail, including the raw materials used and the forming and sintering processes. Although great progress has been made, the development of a high-quality,low-cost fabrication process remains a challenge. Nevertheless, we believe that high-thermal-conductivity silicon nitride substrates are promising for massive practical applications in the next generation of high-power electronic devices.
基金the National Natural Science Foundation of China (No. 50975177)the Shanghai Scienceand Technology Plan of Action for Technical Standardsfor Innovation and Special (No. 08DZ0501700)
文摘The micro-crystalline diamond (MCD) and fine-grained diamond (FGD) films are deposited on commercial silicon nitride inserts by the hot-filament chemical vapor deposition (HFCVD) method. The friction andcutting properties of as-deposited MCD and FGD films coated silicon nitride (Si3N4) inserts are comparatively investigated in this study. The scanning electron microscopy (SEM) and Raman spectroscopy are adopted to studythe characterization of the deposited diamond films. The friction tests are conducted on a ball-on-plate typereciprocating friction tester in ambient air using Co-cemented tungsten carbide (WC-Co), Si3N4 and ball-bearing steel (BBS) balls as the mating materials of the diamond films. For sliding against WC-Co, Si3N4 and BBS,the FGD film presents lower friction coeffcients than the MCD film. However, after sliding against Si3N4, the FGD film is subject to more severe wear than the MCD film. The cutting performance of as-deposited MCD and FGD coated Si3N4 inserts is examined in dry turning glass fiber reinforced plastics (GFRP) composite materials,comparing with the uncoated Si3N4 insert. The results indicate that the lifetime of Si3N4 inserts can be prolonged by depositing the MCD or FGD film on them and the FGD coated insert shows longer cutting lifetime than the MCD coated one.
基金the National Key Research and Development Program of China(2021YFA1401000,2021YFB2801600,and 2017YFF0206104)National Natural Science Foundation of China(62075114 and 62175121)the Beijing Natural Science Foundation(4212050)。
文摘Kerr frequency combs have been attracting significant interest due to their rich physics and broad applications in metrology,microwave photonics,and telecommunications.In this review,we first introduce the fundamental physics,master equations,simulation methods,and dynamic process of Kerr frequency combs.We then analyze the most promising material platform for realizing Kerr frequency combs—silicon nitride on insulator(SNOI)in comparison with other material platforms.Moreover,we discuss the fabrication methods,process optimization as well as tuning and measurement schemes of SNOI-based Kerr frequency combs.Furthermore,we highlight several emerging applications of Kerr frequency combs in metrology,including spectroscopy,ranging,and timing.Finally,we summarize this review and envision the future development of chip-scale Kerr frequency combs from the viewpoint of theory,material platforms,and tuning methods.
基金This work was supported by the National Natural Science Foundation of China(Grant Nos.11504435 and 62171478)the Natural Science Foundation of Hubei Province,China(No.2020CFB450).
文摘The slab effective index difference between the transverse-electric(TE)and transverse-magnetic(TM)polarizations was utilized to obtain complete photonic bandgap(CPBG)in a silicon nitride(Si_(x)N_(y))photonic crystal slab.For this,coincident frequency range in the TE photonic bandgap(PBG)and TM PBG,which denotes the CPBGs of the slab,must be found with the same structure.Through adjusting the effective index pair of TE and TM polarizations by changing the thickness of the Si_(x)N_(y)core layer,and also optimizing the structure parameters within the photonic crystal plane,a large normalized CPBG of 5.62%was theoretically obtained in a slab of Si_(x)N_(y)with a refractive index of 2.5.Moreover,based on the obtained CPBG,a microcavity which could support both TE and TM polarization was theoretically demonstrated.The cavity modes for different polarizations were both well confined,which proved the reliability of the CPBG.In addition,using the same method,the lowest refractive index of Si_(x)N_(y)on silica slab for a CPBG could be extended to as low as 2.The results indicate that there is potential for development of various high-performance CPBG devices based on Si_(x)N_(y)slab technology.
文摘Steam oxidation resistance of Si3N4 and Si2N2O as well as SiAlON bonded SiC refractories at 900℃was tested according to ASTM-C863.Phase composition and microstructure before and after oxidation were analyzed by XRD and SEM.The results show that Si3N4 and Si2N2O bonded SiC refractory presents better steam oxidation resistance than SiAlON bonded SiC.For Si3N4 and Si2N2O bonded SiC,the oxidation speed is higher with more pronounced volume expansion in the early 100 h;afterwards,the volume expansion slows down gradually and starts to level off after 300 h.It is considered that the high silica glass phase formed during the oxidation covers Si3N4 and Si2N2O,and SiC as a protective layer and fills the open pores.But for SiAlON bonded SiC,the volume expands gradually and constantly with the increasing oxidation duration even after 500 h,due to the continuous formation of mullite transformed from oxidation products and Al2O3 in SiAlON.
基金supported by the National Natural Science Foundation of China(U20A20239)the Natural Science Foundation of Hubei Province(2020CFB692)the Scientific Research Fund of Hunan Provincial Education Department(18A428).
文摘In order to investigate the effect of the catalyst loading mode on the mechanical properties of Si_(3)N_(4) composite MgO-C refractories prepared by nitridation,fused magnesia,flake graphite,silicon powder,and phenolic resin were used as the main raw materials,and ferric nitrate as the catalyst to prepare refractories by nitriding at 1350℃.The effects of different catalyst supports(silicon powder,silicon powder+phenolic resin)on the formation of Si_(3)N_(4) in MgO-C refractories and the properties of refractories were studied.The results show that the silicon powder+resin catalyst support promotes the participation ofα-Si_(3)N_(4) in the reaction to generateβ-Si_(3)N_(4) and MgSiN_(2),and generates more SiC.However,this loading mode causes more gas to escape from the refractories and loosens the material structure,which reduces the mechanical properties.On the contrary,MgO-C refractories prepared by nitridation with silicon powder-supported catalysts under the same conditions show higher density and better mechanical properties.
基金Supported by National Natural Science Foundation of China(Grant No.51205097)China Postdoctoral Science Foundation(Grant No.2013M541401)
文摘Laser assisted machining is an effective method to machine advanced materials with the added benefits of longer tool life and increased material removal rates. While extensive studies have investigated the machining properties for laser assisted milling(LAML),few attempts have been made to extend LAML to machining parts with complex geometric features. A methodology for continuous path machining for LAML is developed by integration of a rotary and movable table into an ordinary milling machine with a laser beam system. The machining strategy and processing path are investigated to determine alignment of the machining path with the laser spot.In order to keep the material removal temperatures above the softening temperature of silicon nitride, the transformation is coordinated and the temperature interpolated, establishing a transient thermal model. The temperatures of the laser center and cutting zone are also carefully controlled to achieve optimal machining results and avoid thermal damage. These experiments indicate that the system results in no surface damage as well as good surface roughness, validating the application of this machining strategy and thermal model in the development of a new LAML system for continuous path processing of silicon nitride. The proposed approach can be easily applied in LAML system to achieve continuous processing and improve efficiency in laser assisted machining.
