Evaluation of processing parameters effects on the formation of Si3N4 wires synthesized by means of ball milling and nitridation route

Crystalline silicon nitride (Si₃N₄) wires have been synthesized by means of ball milling and nitridation route. The influence of temperature of reaction and starting condition of the powder (milled or unmilled) on the synthesis of Si₃N₄ wires were studied. The reduced size of silicon particle during the milling process led to an increased degree of nitridation.Silicon powders with higher surface energy can react incessantly with nitrogen to form silicon nitride wires. The results show that the Si₃N₄ was fully formed with two kinds morphologies including globular and wire with a width of 100–300 nm and a length of several microns at temperature of 1300 °C for 1 h by employing the milled silicon powder. The infrared adsorption of wires exhibit absorption bands related to the absorption peaks of Si–N band of Si₃N₄.     

Fabrication,mechanical properties and microstructure analysis of Si3N4/SiC nanocomposite

Ceramic nanocomposites, Si₃N₄ matrix reinforced with nano-sized SiC particles, were fabricated by hot pressing the mixture of Si₃N₄ and SiC fine powders with different sintering additives. Distinguishable increase in fracture strength at low and high temperatures was obtained by adding nano-sized SiC particles in Si₃N₄ with Al₂O₃ and/or Y₂O₃. Si₃N₄/SiC nanocomposite added with Al₂O₃ and Y₂O₃ demonstrated the maximum strength of 1.9 GPa with average strength of 1.7 GPa. Fracture strength of room temperature was retained up to 1400 as 1 GPa in the sample with addition of 30 nm SiC and 4 wt% Y₂O₃. Striking observation in this nanocomposite is that SiC particles at grain boundary are directly bonded to Si₃N₄ grain without glassy phases. Thus, significant improvement in high temperature strength in this nanocomposite can be attributed to inhibition of grain boundary sliding and cavity formation primarily by intergranular SiC particles, besides crystallization of grain boundary phase.     

Spark plasma sintering of silicon nitride using nanocomposite particles

The spark plasma sintering (SPS) of silicon nitride (Si₃N₄) was investigated using nanocomposite particles composed of submicron-size α-Si₃N₄ and nano-size sintering aids of 5 wt% Y₂O₃ and 2 wt% MgO prepared through a mechanical treatment. As a result of the SPS, Si₃N₄ ceramics with a higher density were obtained using the nanocomposite particles compared with a powder mixture prepared using conventional wet ball-milling. The shrinkage curve of the powder compact prepared using the mechanical treatment was also different from that prepared using the ball-milling, because the formation of the secondary phase identified by the X-ray diffraction (XRD) method and liquid phase was influenced by the presence of the sintering aids in the powder compact. Scanning electron microscopy (SEM) observations showed that elongated grain structure in the Si₃N₄ ceramics with the nanocomposite particles was more developed than that using the powder mixture and ball-milling because of the enhancement of the densification and α-β phase transformation. The fracture toughness was improved by the development of the microstructure using the nanocomposite particles as the raw material. Consequently, it was shown that the powder design of the Si₃N₄ and sintering aids is important to fabricate denser Si₃N₄ ceramics with better mechanical properties using SPS.     

A novel fiber-reinforced polyethylene composite with added silicon nitride particles for enhanced thermal conductivity

A novel thermally conductive plastic composite was prepared from a mixture of silicon nitride (Si₃N₄) filler particles and an ultrahigh molecular weight polyethylene–linear low density polyethylene blend. The effects of Si₃N₄ particle sizes, concentration, and dispersion on the thermal conductivity and relevant dielectric properties were investigated. With proper fabrication the Si₃N₄ particles could form a continuously connected dispersion that acted as the dominant thermally conductive pathway through the plastic matrix. By adding 0–20% Si₃N₄ filler particles, the composite thermal conductivity was increased from 0.2 to ～1.0 W m^?1 K^?1. Also, the composite thermal conductivity was further enhanced to 1.8 W m^?1 K^?1 by decreasing the Si₃N₄ particle sizes from 35, 3 and 0.2 μm, and using coupling agent, for the composites with higher filler content. Alumina short fibers were then added to improve the overall composite toughness and strength. Optimum thermal, dielectric and mechanical properties were obtained for a fiber-reinforced polyethylene composite with 20% total alumina–Si₃N₄ (0.2 μm size) filler particles.     

Joining of AlN and graphite disks using interlayer tapes by spark plasma sintering

AlN and graphite disks were successfully joined using a polymer plasticized ceramic tape as the interlayer by spark plasma sintering (SPS). The tape contains either composite powders of AlN and graphite or AlN powders without graphite. Both tapes contained 5 mass% Y₂O₃ as the sintering aid of AlN. The joining was carried out at 1700–1900 °C and 30 MPa for 5 min. No other reaction phase except for Al₂Y₄O₉ was identified in the joints. The maximum tensile strength of the joints was obtained when the AlN–graphite composite interlayer tape was used. The joining mechanism is attributed not to the chemical bonding, but to the physical bonding of the Al₂Y₄O₉ phase, which is solidified from the molten Al–Y–O squeezing into the porous graphite under pressure during SPS.     

Study on tribological behavior of electrodeposited Cu–Si3N4 composite coatings

Cu–Si₃N₄ composite coatings were prepared by electrolysis from a copper sulphate solution containing dispersed Si₃N₄ particles of 0.4 or 1 μm mean size. Wear behavior of Cu–Si₃N₄ composite and pure copper coatings were evaluated using a pin-on-disc test machine under dry condition sliding. Effects of current density and particle concentration on the incorporation percentage of Si₃N₄, the preferred orientation of copper crystallites, the microstructure, the microhardness and the wear resistance of the coatings were determined. Si₃N₄ particles in the copper matrix resulted in the production of composite deposits with smaller grain sizes and led to change the preferred orientation growth from [1 0 0] to [1 1 0]. It was proved that the presence of Si₃N₄ particles decreases the wear loss and the friction coefficient of the coating. According to the results, the friction coefficient decreased dramatically from 0.52 to 0.26 for pure copper coatings to 0.16–0.24 for Cu–Si₃N₄ composite coatings. In addition, fluctuation of friction coefficient values for Cu–Si₃N₄ composite coating was lower compared with the pure copper coating. The wear properties of Cu–Si₃N₄ composite coatings were shown to depend on the weight fraction, the size and the distribution of co-deposited particles.     

Fabrication of a polymer composite with high thermal conductivity based on sintered silicon nitride foam

A novel route was developed to fabricate Si₃N₄/epoxy composite. In this route, the Si₃N₄ particles were constructed into the foamed shape by using protein foaming method, firstly. Then the Si₃N₄ foams were sintered to bond these Si₃N₄ particles together. Finally, the Si₃N₄/epoxy composite was fabricated by infiltrating the epoxy resin solution into the sintered Si₃N₄ foams. This route was proved to be an efficient way in enhancing the thermal conductivity of epoxy matrix at a low loading fraction. For example, the thermal conductivity of the as-prepared Si₃N₄/epoxy composite with a loading fraction of 22.2 vol% was up to 3.89 W m⁻¹ K⁻¹, which was about 17 times higher than that of neat epoxy.     

Microstructure and properties of porous silicon nitride ceramics prepared by gel-casting and gas pressure sintering

Wave-transparent porous Si₃N₄ ceramics were prepared by gel-casting and gas pressure sintering, and the effects of solid loading on microstructure, mechanical and dielectric properties were investigated. Microstructures with interlocked elongated β-Si₃N₄ grains and uniformly distributed pores were observed, while both the β-Si₃N₄ phase content and grain aspect ratio reduced as the solid loading increased due to the restrained anisotropic growth of β-Si₃N₄ grains. As the solid loading increased from 30 to 45 vol.%, the porosity of ceramics declined from 57.6% to 36.4%. The flexural strength increased linearly from 108.3 to 235.1 MPa, and the dielectric constant and loss tangent of ceramics increased from 2.63 and 2.85 × 10⁻³ to 3.68 and 3.56 × 10⁻³ (10 GHz), respectively.     

Limiting the development of Al4C3 to prevent degradation of Al/SiCp composites processed by pressureless infiltration

The presence of Al₄C₃ in Al/SiC composites may activate degradation of the material by its interaction with water; even moisture may cause its environmental degradation. It has been demonstrated that incorporation of 6 vol% SiO₂ powders into SiC_p preforms before processing by pressureless infiltration prevents formation of Al₄C₃. Analysis by electron back-scattered diffraction confirms that regardless of its crystal structure (α-quartz or α-cristobalite), SiO₂ completely reacts to form MgAl₂O₄. The metal/composite interface microstructure condition of the specimens processed under the most severe conditions (1100 °C for 60 min), four months later confirms the effectiveness of the SiO₂ powders.     

Carbothermal formation and microstrutural evolution of α′-Sialon–AlN–BN powders from boron-rich blast furnace slag

Boron-rich blast furnace slag of low activity is one of the major products created during the separation of iron and boron from ludwigite in a blast furnace process, and the high-efficiency utilisation of its is of great importance to the Chinese boron industry. This paper proposes one new application process to synthesize α′-Sialon–AlN–BN powders by a carbothermal reduction–nitridation method using boron-rich blast furnace slag as the staring material and describes a series of experimental studies that were performed to elucidate the mechanism of phase formation and microstructure evolution during CRN. The experimental results revealed that the phase compositions and microstructures of the synthesized products were greatly affected by the initial compositions ((Ca,Mg)_xSi_12–3xAl_3xO_xN_16–x), x = 0.3–1.8), temperature and holding time. With the compositions shifting from values of x of 0.3–1.8, the relative amount of α′-Sialon, AlN and BN increased gradually, and the amount of α′-Sialon reached a maximum at a value of x of 1.4. The optimal condition for powder synthesis was a temperature of 1480 °C with a holding time of 8 h, under which the crystalline phases included α′-Sialon, AlN, BN and less SiC. More elongated α′-Sialon grains were observed at higher x values and temperatures. During the CRN process, MgAl₂O₄, Mg₂SiO₄, Ca₂Al₂SiO₇, MgSiN₂, β′-Sialon and 27R appeared sequentially as intermediate products. The volatilisation of SiO gas and magnesium vapour resulted in additional weight loss of the samples, which was aggravated with increases in the synthesis temperature and holding time.     

Preparation of TiN–Ti5Si3 in-situ composites by Selective Laser Melting

The Selective Laser Melting (SLM) Rapid Manufacturing (RM) of the high-energy ball milled Ti–Si₃N₄ composite powder with the mol ratio of 9:1 was performed in the present work. The microstructural characterizations revealed the formation of TiN reinforced Ti₅Si₃ matrix composites after laser processing via the in-situ synthesis reaction 9Ti + Si₃N₄ = 4TiN + Ti₅Si₃. The in-situ presented TiN reinforcing phase possessed a refined granular morphology and a uniform distribution throughout the Ti₅Si₃ matrix, showing a clear and compatible interfacial structure with the matrix. The metallurgical mechanisms for the in-situ synthesis of TiN reinforced Ti₅Si₃ matrix composites by SLM were also proposed.     

Tribological behavior of Ni3Al matrix self-lubricating composites containing WS2, Ag and hBN tested from room temperature to 800 °C

Ni₃Al matrix self-lubricating composites (NMSC) containing varied amounts of WS₂, Ag and hBN (WAh) with weight ratio of 1:1:1 were fabricated by in situ technique using spark plasma sintering. The friction and wear properties of NMSC against the commercial Si₃N₄ ceramic ball at the load of 10 N and sliding speed of 0.234 m/s for 80 min from room temperature to 800 °C were investigated. The results showed that the tribological properties of NMSC strongly depended on the addition content of WAh. Moreover, NMSC with 15 wt.% WAh and 5 wt.% TiC exhibited the relatively lower friction coefficients and the less wear rates from RT to 800 °C. The excellent tribological behavior of NMSC with 15 wt.% WAh and 5 wt.% TiC was attributed to the synergetic action of composite lubricants of WAh and reinforced phase of TiC.     

Microstructure and properties of the Si3N4/silica aerogel composites fabricated by the sol–gel method via ambient pressure drying

Si₃N₄ particle reinforced silica aerogel composites have been fabricated by the sol–gel method via ambient pressure drying. The microstructure and mechanical, thermal insulation and dielectric properties of the composites were investigated. The effect of the Si₃N₄ content on the microstructure and properties were also clarified. The results indicate that the obtained mesoporous composites exhibit low thermal conductivity (0.024–0.072 Wm^− 1 K^− 1), low dielectric constant (1.55–1.85) and low loss tangent (0.005–0.007). As the Si₃N₄ content increased from 5 to 20 vol.%, the compressive strength and the flexural strength of the composites increased from 3.21 to 12.05 MPa and from 0.36 to 2.45 MPa, respectively. The obtained composites exhibit considerable promise in wave transparency and thermal insulation functional integration applications.     

Thermal stability of magnetron sputtered Si–B–C–N materials at temperatures up to 1700 °C

Thermal stability of deposited Si–B–C–N materials (film fragments or powders without a substrate) in inert gases (He and Ar) up to 1700 °C was investigated using differential scanning calorimetry, high-resolution thermogravimetry and X-ray diffraction measurements. Amorphous Si–B–C–N films were fabricated by dc magnetron co-sputtering of a single B₄C–Si target in two nitrogen–argon gas mixtures (50% N₂ + 50% Ar or 25% N₂ + 75% Ar). It was found that the deposited Si–B–C–N materials can be more stable at high temperatures in the inert atmosphere than the usually used substrates (e.g. SiC or BN). The materials with the compositions (in at.%) Si_32–33B₁₀C₂N_50–51, for which N/(Si + B + C) = 1.1–1.2, retained their amorphous structure up to 1600 °C without any structural transformations and detectable mass changes.     

Formation of a single-phase Ti3AlC2 from a mixture of Ti,Al and TiC powders with Sn as an additive

A high purity of Ti₃AlC₂ powder has been synthesized by pressureless sintering a mixture of Ti/Al/TiC/Sn (Sn as a sintering additive) powders with a mole ratio of 1:1:1:0.1 in the temperature range of 1350–1500 °C for 10 min in an Ar atmosphere. Sn is an effective additive and its effect on the formation of Ti₃AlC₂ has been discussed. The formation mechanism of Ti₃AlC₂ has been proposed. X-ray diffraction analysis and scanning electron microscopy were used to characterize the samples.     

Influence of yttrium dopant on the synthesis of ultrafine AlN powders by CRN route from a sol–gel low temperature combustion precursor

Y-doped ultrafine AlN powders were synthesized by a carbothermal reduction nitridation (CRN) route from precursors of Al₂O₃, C and Y₂O₃ prepared by a sol–gel low temperature combustion technology. The Y dopant reacted with alumina and thus forming yttrium aluminate of AlYO₃, Al₃Y₅O₁₂ and Al₂Y₄O₉, which formed a liquid at about 1400 °C and promoted the transformation of Al₂O₃ to AlN and the growth of AlN particles. Compared with the conventional solid CRN process, Y dopant reduced the synthesis temperature by 150 °C, and Al₂O₃ transformed to AlN completely at 1450 °C. The content of Y dopant had little effect on the synthesis temperature of AlN whereas it influenced the phase of Y compounds in the products. As the Y/Al molar ratio was in the range of 0.007648–0.022944, the particle sizes of Y-doped AlN powders synthesized at 1450 °C were 150–300 nm.     

Powder synthesis and properties of LiTaO3 ceramics

The LiTaO₃ powders with sub micrometer grade grain size have been synthesized successfully using a molten salt method. Lithium tantalate began to form at 400 °C reaction temperature and transformed to pure phase without residual reactants when it was processed at 500 °C for 4 h in static air. The undoped LiTaO₃ ceramics with a Curie temperature about 663 °C were obtained by pressureless sintering at 1300 °C for 3 h. The relative dielectric constant (ɛ_r) increases from 50 to 375 at temperature ranging from 30 to 663 °C and then decreases quickly as the temperature increases above 663 °C. The ceramics shows a relative dielectric constant of 49.4, a dielectric loss factor (tan δ) of 0.007, a coercive field (Ec) of 28.66 kV/cm and a remnant polarization (Pr) of 32.48 μC/cm² at room temperature.     

Preparation of YAG gel coated ZrB2–SiC composite prepared by gelcasting and pressureless sintering

In this paper, gelcasting and pressureless sintering of YAG gel coated ZrB₂–SiC (YZS) composite were conducted. YAG gel coated ZrB₂–SiC (YZS) suspension was firstly prepared through sol–gel route. Poly (acrylic acid) was used as dispersant. YZS suspension had the lowest viscosity when using 0.6 wt.% PAA as dispersant. Gelcasting was conducted based on AM–MBAM system. The gelcast YZS sample was then pressureless sintered to about 97% density. During sintering, YAG promoted the densification process from solid state sintering to liquid phase sintering. The average grain sizes of ZrB₂ and SiC in the YZS composite were 3.8 and 1.3 μm, respectively. The flexural strength, fracture toughness and microhardness were 375 ± 37 MPa, 4.13 ± 0.45 MPa m^1/2 and 14.1 ± 0.5 GPa, respectively.     

Sinter-HIP of polymer-derived Al2O3–SiC composites with high SiC contents

Submicrometer Al₂O₃ composites with more than 20 vol.% of SiC particles were produced using a multiple infiltration of porous bodies with a liquid polymer SiC precursor. The fully dense composites were successfully densified using a sinter-HIP process. Parameters of sintering and HIP steps are discussed with respect to both densification and microstructure evolution of the composites. The initial pressure during the sintering step plays an important role for the preparation of fully dense composites with a submicrometer alumina matrix at 1750 °C. Optimized densification schedule of sinter-HIP represents a novel approach of densification at relatively mild conditions compared to previously reported or common densification methods of Al₂O₃–SiC composites with high SiC content, such as pressureless sintering, hot pressing and post-HIPing. The method expands the possibilities for preparation of alumina based composites with SiC volume fraction > 20 vol.%, filling the gap in available literature data.     

Vacuum-UV excitation and visible luminescence of nano-scale and micro-scale NaLnF4:Pr3+ (Ln = Y,Lu)

The UV–Vis luminescence of NaLnF₄:Pr³⁺ (Ln = Y, Lu) materials can be efficiently excited by vacuum UV radiation (VUV) such as the 172 nm emission of mercury-free Xe-discharge lamps. In this work, the optical properties of the cubic α-phase and the hexagonal β-phase of NaLnF₄:Pr³⁺ (Ln = Y, Lu) powders are compared regarding particle sizes in the nano- and micrometer regime. Upon VUV excitation, the emission spectra of both crystal phases are found to be dominated by intraconfigurational [Xe]4f²–[Xe]4f² transitions, which is explained by the chemical properties of the ternary fluorides. Furthermore it is observed that the emission and excitation spectra of nano- and micro-scale powders are very similar, but that the luminescence intensity is affected by the average particle size.