Polymer/filler derived NbC composite ceramics

NbC containing ceramic composites were manufactured from poly(siloxane)/Nb/NbC filler mixtures by a high temperature reaction bonding process. During heating in an inert atmosphere the Si—O—C ceramic residue of the polymer reacted with the metallic Nb filler to form Nb _x Si _y , NbO and NbC. Samples with a high Nb/NbC ratio showed reduced porosity and increased hardness after pyrolysis at 1200°C.     

Niobium boride coating on AISI M2 steel by boro-niobizing treatment

In this study, niobium boride coating was applied on pre-boronized AISI M2 steel by the thermo-reactive deposition technique in a powder mixture consisting of ferro-niobium, ammonium chloride and alumina at 950 °C for 1-4 h. The coated samples were characterized by X-ray diffraction, scanning electron microscope and micro-hardness tests. Niobium boride layer formed on the pre-boronized AISI M2 steel was smooth, compact and homogeneous. X-ray studies showed that the phases formed on the steel surfaces are NbB, Nb₃B₂, FeB and Fe₂B. The depth of the niobium boride layer ranged from 0.97 μm to 3.25 μm, depending on treatment time. The higher the treatment time the thicker the niobium boride layer observed. The hardness of the niobium boride layer was 2738 ± 353 HV_0.01.     

Facile synthesis,characterization and photocatalytic activity of niobium carbide

Niobium carbide (NbC) powders were prepared via a novel route at 550 °C and 8 h, using metallic magnesium powders, niobium pentoxide (Nb₂O₅), and potassium acetate (CH₃COOK) as starting materials. The structure and morphology of the product were characterized by X-ray powder diffraction (XRD) and scanning electron microscopy (SEM). The results indicated that as-prepared product was crystallized in pure cubic NbC phase and the size of the sample was estimated to be around 120 nm. The Rietveld refinement of the XRD data gives the cell constant a = 4.4718 Å. According to the Scherrer formula, the real grain size was about 70 nm. The BET surface area of the sample was ca.29.3 m²/g. The grain size distribution of the sample was about 467 nm, which was characterized by N4 PLUS submicron Particle Size Analyzer. The cubic NbC powders exhibited photocatalytic activity in degradation of Rhodamine-B (RhB) under 300 W mercury lamp light irradiation.     

Dielectric properties of Lanxide™ Al2O3/Al composites

The dielectric properties of unreinforced Lanxide Al₂O₃/Al composites have been investigated over a wide range of temperatures and frequencies. These composites were formed by the directed oxidation of suitably doped aluminium-based alloy melts, with no filler or reinforcing material in the reaction path. As-grown composite materials were good electrical conductors in all directions owing to the presence of an interconnected metallic constituent. As the metallic phases were partially removed (in favour of porosity) by continuing the oxidation reaction to completion, the composites remained electrically conducting parallel to, and became insulating transverse to, the original growth direction of the composite. This anisotropy apparently was caused by different connectivity of the metal phase between the two directions. Thermal treatments at 1600°C in argon resulted in volatilization of the residual metal in the composite, thus further increasing the porosity. As the metal content was decreased, the composites changed from conducting to insulating along the growth direction. When the metallic phase was removed completely, the porous alumina ceramic maintained anisotropic dielectric properties, due to c-axis alignment of the alumina (corundum) phase along the growth direction. The dielectric constants were 8.0 and 6.4, respectively, parallel and perpendicular to the c-axis aligned directions of the porous alumina ceramic. A dielectric relaxation phenomenon was observed in some samples of both as-grown and thermally treated material, and was attributed to an unidentified impurity effect.     

The preparation and properties of biodegradable polyesteramide composites reinforced with nano-CaCO3 and nano-SiO2

Composites were fabricated utilizing melt mixing aliphatic polyesteramide (PEA) with ordinary CaCO₃, nano-CaCO₃, and nano-SiO₂. The effect of filler on the matrix was studied by mechanical properties and hydrolysis rate measuring. The ordinary filler as well as the nano-filler had a negative effect on the stability of the polymer melt, and an improved mechanical property was obtained around a critical concentration of the filler where a percolation phenomenon appeared. When the composites underwent hydrolysis, the inert filler played a role as a mechanical obstacle in the matrix and retarded the hydrolysis; on the other hand, the interfacial area between the filler particle and the matrix resin increased with the filler, which would accelerate the hydrolysis. As a result of these two inverse effects, a minimum and a maximum value appeared in the plot of the degradation rate-filler content graph. For the ordinary filler filled polymer, the filler retarded the hydrolysis; in great contrast, the hydrolysis rate of nano-composites showed a maximum value around the critical concentration of the filler, and was much higher than the neat resin.     

The effect of polysiloxane on the properties of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-NbC composite material produced by pyrolysis process

Recently, studies have been developed in order to obtain Al₂O₃-NbC composite materials. The reinforced materials have shown good potential to be used as cutting tool materials at high-speed cutting and high temperature as a substitute to WC-Co material. The main disadvantage to produce these alumina-reinforced materials is the necessity to use pressure assisted sintering or high sintering temperatures to produce dense bodies. Manufacturing of composite ceramic materials derived from polymer reactive filler has been intensively investigated. Polymer pyrolysis is a relatively new and very promising method for obtaining ceramic material in complex shapes and lower sintering temperatures. This work investigated a ceramic composite matrix based in SiC_xO_y and Al₂O₃ and reinforced with NbC obtained by means of the active fillers pyrolysis process. The results obtained in this work demonstrate that using a mixture of polysiloxanes produces a composite material with better properties when compared to others polymer materials.     

AC electrical and optical characterization of epoxy–Al2O3 composites

The AC electrical and optical characterizations of epoxy–alumina (Al₂O₃) composites have been investigated. Sheets filled with alumina were prepared with different alumina concentrations (0, 2, 5, 8, 10, and 15 wt%). The AC electrical properties were measured by using impedance spectroscopy as a function of applied frequency in range from 50 kHz to 1 MHz and filler concentration. The results obtained showed that the applied frequency and filler concentration was found to influence the AC electrical conductivity and dielectric behavior of the prepared composites. The UV-optical results obtained were analyzed in terms of the absorption formula for non-crystalline materials. The absorption coefficient and the optical energy gap (E_opt) have been obtained from the direct allowed transitions in k-space at room temperature. The tail widths (ΔE) of the localized states in the band gap were evaluated using the Urbach-edges formula. It was found that both (E_opt) and (ΔE) vary with the alumina concentration dispersed in the epoxy matrix. The refractive index (n) for the composites was determined from the collected transmittance and reflectance spectra. The dispersion behavior of the refractive index is discussed in terms of the single oscillator model.     

Densification, phase composition, and properties of borosilicate glass composites containing nano-alumina and titania

Five samples of glass/ceramic composites were prepared from borosilicate glasses and both nano-aluminum oxide and nano-titanium oxide. The glass composite samples contain 10, 20, 30, 40, 50 wt.% of alumina and titania mixture. The ratio of Al₂O₃:TiO₂ in the mixture was 1:1. The formation of cristobalite in the glass matrix of low firing glass/ceramic composite substrates limits the efficiency of the ceramic substrate when it is used in circuit boards. In the present study, addition of both alumina and titania to a borosilicate glass as a ceramic filler caused the diffusion of alumina and titania phases (anatase and rutile) constituents into the glass matrix and prevented the formation of a cristobalite. Addition of both the ceramics suppresses cristobalite formation more effectively than one of them used alone and results in lower dielectric constant and thermal expansion coefficients.     

废印刷电路板非金属粉负载二氧化硅杂化填料的制备及其在不饱和聚酯中的应用

为增强废印刷电路板非金属粉(WPCBP)与聚合物基体之间的界面结合作用,采用溶胶-凝胶法在WPCBP表面原位负载了一层纳米二氧化硅粒子(SiO_2),制备了一种新型的WPCBP-SiO_2杂化填料。SEM、TGA和FTIR证明SiO_2通过化学键成功负载到了杂化填料的表面。采用含双键的界面改性剂对杂化填料进行改性后,应用于不饱和聚酯树脂基体,探讨了未改性杂化填料及表面改性杂化填料对不饱和聚酯复合材料的力学性能、界面结合作用和热稳定性能的影响。结果表明,新型的杂化填料WPCBP-SiO_2能够与不饱和聚酯基体形成强的界面结合作用,显著提高不饱和聚酯复合材料的力学性能和热稳定性能,且表面改性后复合材料的各项性能得到进一步提高。     

Inter-diffusion of carbon into niobium coatings deposited on graphite

The inter-diffusion of carbon (originating from a graphite substrate) into a niobium coating and the fabrication of its carbides by heat treatment in the temperature range of 1073-1773 K was studied. The thickness of the Nb₂C and NbC phases formed after heat treatment as well as the inter-diffusion coefficients for the formation of the carbide layers were also studied. It was found that the carbide layer growth displayed parabolic behavior patterns inherent in the growth rate constants (K) of Nb₂C and NbC layers.By assuming that the inter-diffusion coefficients are independent of concentration, it was possible to determine the inter-diffusion coefficients of carbon D^c into Nb₂C and NbC layers as a function of temperature.     

Ceramic matrix composites derived from CrSi2-filled silicone polycyclic network

Ceramic matrix composites (CMC) were prepared by the active-filler-controlled polymer pyrolysis, using a siloxane polycyclic network filled with CrSi₂. The starting CrSi₂-filled polysiloxane was pyrolyzed in both nitrogen and argon atmospheres, up to 1450°C. During the pyrolysis in nitrogen atmosphere, the CrSi₂ particles reacted with N₂, and also with carbon from the preceramic polymer binder, still complete consumption of the filler particles. Such reactions led to a dramatic change in the composition and microstructure of the resulting ceramic monoliths, which displayed linear expansion of 1.7%. In argon atmosphere, the CrSi₂ particles acted as inert filler during the pyrolysis process. The final CMC compositions obtained in N₂ and Ar atmospheres were Cr_0.62C_0.25N_0.03-Si₃N₄-Cr₃C₂ and SiO_xC_y-SiC-CrSi₂, respectively.     

Effect of different binders and secondary carbides on NbC cermets

Due to the rapidly increasing price of tungsten carbide and the significant health risks associated with the wear products of WC-Co (Co₃O₄ and Wo₃), an alternative is required. Niobium carbide (NbC) is well suited as a cutting tool due to its high melting point and low solubility in iron. Compared to pure NbC, a complete substitution of WC to NbC-Co resulted in an increased toughness and strength. As alternative binders, nickel and iron-based binders were subsequently investigated. Although iron-based cermets would be an economical, low-cost alternative to NbC-Ni cermets, they showed a higher coefficient of friction and wear rate. So far, NbC-Ni cermets best met the requirements of high hardness and toughness. Various secondary carbides such as VC, Mo₂C, TiC, but also WC were added to further improve the hardness. Elemental analyses of NbC-Ni-MeC cermets (Me = metal) showed that the binder is a face-centered cubic solid solution, while the NbC phase is a solid solution of the type (Nb, Me)C.

     

Silicide characterization at alumina–niobium interfaces

Alumina–niobium interfaces formed by liquid-film-assisted joining with copper/niobium/copper interlayers exhibited microstructures that depend on the nature of the alumina components. Characterization of these interfaces in the transmission electron microscope provided insight on the relationship between interfacial microstructure and fracture performance. Interfaces between sapphire and niobium and those between high-purity (99.9%) polycrystalline alumina and niobium were free of secondary phases. However, niobium silicides were found at interfaces between lower-purity (99.5%) alumina and niobium, identified by electron diffraction analysis as the body-centered tetragonal α-Nb₅Si₃ phase. Spatially resolved compositional analysis was conducted on silicide particles at and away from the interface.     

Synthesis,microstructure and mechanical properties of Al2O3 reinforced Ni3Al matrix composite

A new method to synthesize alumina reinforced Ni₃Al intermetallic matrix composites has been described. The powder mixture of nickel and aluminium was mechanically alloyed. The powder mixture was excessively heated during mechanical alloying and then exposed to atmosphere for oxidation. The oxidized powder mixture was transformed into alumina reinforced nickel aluminide matrix composite on subsequent pulse current processing. Alumina reinforcements were generated in the nickel aluminide matrix by in situ precipitation. The microstructure of the composite showed that the alumina reinforcements were 50–150 nm in size. The fine alumina reinforcements were homogeneously distributed in the matrix phase. The mechanical properties of the alumina reinforced nickel aluminide matrix composite fairly exceeded the nickel aluminide alloys. This novel synthesis approach allowed the rapid and facile production of high strength alumina reinforced Ni₃Al matrix composites.     

The effect of interfacial state on the thermal conductivity of functionalized Al2O3 filled glass fibers reinforced polymer composites

Rapidly increasing packaging density of electronic devices puts forward higher requirements for thermal conductivity of glass fibers reinforced polymer (GFRP) composites, which are commonly used as substrates in printed circuit board. Interface between fillers and polymer matrix has long been playing an important role in affecting thermal conductivity. In this paper, the effect of interfacial state on the thermal conductivity of functionalized Al₂O₃ filled GFRP composites was evaluated. The results indicated that amino groups-Al₂O₃ was demonstrated to be effective filler to fabricate thermally conductive GFPR composite (1.07 W/m K), compared with epoxy group and graphene oxide functionalized Al₂O₃. It was determined that the strong adhesion at the interface and homogeneous dispersion of filler particles were the key factors. Moreover, the effect of interfacial state on dielectric and thermomechanical properties of GFRP composites was also discussed. This research provides an efficient way to develop high-performance GFRP composites with high thermal conductivity for integrated circuit packaging applications.     

Modelling of dimensional changes during polymer-ceramic conversion for bulk component fabrication

Shrinkage and porosity generation during conversion of polymer-filler systems into ceramic bodies during pyrolysis is examined. In the presence of an inert filler phase such as Si₃N₄ or SiC powder dispersed in an organosilicon polymeric matrix only porous microstructures may be obtained without any shrinkage. By using an active filler phase such as carbide- or nitride-forming transition metals, however, shrinkage of the polymer matrix may be compensated by appropriate expansion of the filler phase. A model is derived to predict the critical volume fractions of various potential active filler systems in inert and reactive gas atmospheres, which can be effective in controlling shrinkage and porosity during the fabrication of ceramic components from polymer-derived precursor materials.Nomenclature P Polymer phase - C Condensed polymer pyrolysis product (ceramic) - G Gaseous polymer decomposition product - F Inert filler phase - T Active filler phase (e.g. transition metal) - M Reaction product of active filler phase (e.g. carbide, nitride) - m Mass - V Volume fraction - V _F,T ^max Maximum packing density of an inert (F) or active (T) filler powder - V _F,t ^* Critical volume fraction of an inert (F) or active (T) filler powder in the starting polymer-filler mixture - V _v Residual porosity in the polymer pyrolysis product - V _v ^pf Residual porosity in the polymer-inert filler system after pyrolysis - Ceramic yield of polymer after pyrolysis - Weight change of active filler phase during reaction pyrolysis - Density ratio of polymer to polymer pyrolysis (ceramic) product - Density ratio of active filler to filler reaction product - ^P Linear shrinkage of the polymer phase during pyrolysis - ^pf Linear shrinkage of a polymer-inert filler system during pyrolysis - ^paf Linear shrinkage of a polymer-active filler system during reaction pyrolysis - Linear shrinkage/expansion of the filler phase during reaction - Density     

Enhanced thermal conductivity of epoxy nanocomposites filled with hybrid filler system of triethylenetetramine-functionalized multi-walled carbon nanotube/silane-modified nano-sized silicon carbide

Multi-walled carbon nanotubes (MWCNTs) were first treated by a 3:1 (v/v) mixture of concentrated H₂SO₄/HNO₃, and then triethylenetetramine (TETA) grafting was carried out. Nano-sized silicon carbide particles (SiC_np) were modified by the silane coupling agent. Epoxy nanocomposites filled with hybrid filler system containing TETA-functionalized MWCNTs and silane-modified SiC_np were prepared. The investigation on the thermal conductivity of epoxy nanocomposites filled with single filler system and hybrid filler system was performed. Chemical surface treatment is conducive to the enhancement of thermal conductivity of epoxy composites. The thermal conductivity of epoxy composites with hybrid filler system is higher than that of epoxy composites with any single filler system (functionalized MWCNTs or modified SiC_np), which is due to the effective combination of MWCNT-to-MWCNT and SiC_np-to-SiC_np conductive networks. Hybrid filler system could provide synergistic effect and cost reduction simultaneously.     

Dielectric,thermal and mechanical properties of Sr<Subscript>2</Subscript>ZnSi<Subscript>2</Subscript>O<Subscript>7</Subscript> based polymer/ceramic composites

Polymer/Sr₂ZnSi₂O₇ (SZS) ceramic composites suitable for substrate applications have been developed using the polymers polystyrene (PS), high density polyethylene (HDPE) and Di-Glycidyl Ether of Bisphenol A (DGEBA). The dielectric, thermal and mechanical properties of the composites are investigated as a function of various concentrations of the ceramic filler. The obtained values of relative permittivity, dielectric loss tangent, thermal conductivity and coefficient of thermal expansion of the composites are compared with the corresponding theoretical predictions. The relative permittivity of the polymer/ceramic composites increases with filler loading. The dielectric loss tangent also shows the same trend except for DGEBA/SZS composites. The major advantages of the ceramic loading are improvement in thermal conductivity and a decrease in the coefficient of thermal expansion. The tensile strength of the composites decreases with increase in filler content, whereas an improvement is observed in microhardness. The variation of relative permittivity (at 1 MHz) of the composites is also studied as a function of temperature.     

Microstructure and mechanical properties of chromium and chromium/nickel particulate reinforced alumina ceramics

A range of Al₂O₃-Cr and Al₂O₃-Cr/Ni composites have been made using either pressureless sintering in the presence of a graphite bed or hot pressing. Examination of the microstructures shows that they are fully dense (typically 98–99% of the theoretical density) and that the micrometre-scale metallic particles remain discrete and homogeneously dispersed in all composites. All of the hot pressed specimens had higher flexural strengths than the sintered materials. Within each processing route, the composites had slightly lower strength values than the equivalent monolithic alumina specimens. This was attributed to weak interfacial bonding. Fracture toughness behaviour was investigated using indentation and double cantilever beam methods. All of the composites were found to be tougher than the parent alumina and to show resistance-curve behaviour. For the composites, maximum fracture toughness values were 5–6 MPa m^1/2 (about double the value for alumina) for process zone sizes of a few millimetres, although steady state was not reached in the limited number of specimens tested. Examination of fracture surfaces and indentation cracks showed that the toughening potential of the metal particles was not exploited to any significant extent. This was mainly due to weak metal-Al₂O₃ interfaces, but also because of carbon embrittlement of the metallic particles in which chromium was the major constituent.     

The effects of β-alumina on the production of Al2O3/Al composites by the directed melt oxidation process

Directed melt oxidation (DMOX) of pure aluminium has been used to produce Al/Al₂O₃ composites by growth into a particulate alumina filler in the absence of any dopants apart from a -Al₂O₃ impurity in the filler. The microstructural development and mechanisms of growth of these composites have been investigated. It is shown that the Al₂O₃ filler used in this work has both chemical and physical effects on the reaction process. The -Al₂O₃ impurity introduces sodium into the system; this increases the wettability of alumina (both filler and oxidation reaction product) by molten aluminium, and initiates DMOX reactions. In addition, the filler particle size has an effect on the directed oxidation reaction. If the particle size is too fine, no oxidation growth takes place. Filler particles limit the ingress of oxygen through the reaction front so that AIN instead of Al₂O₃ may be formed in regions behind the main reaction front. Although such AIN production is seen when magnesium is used as a dopant to initiate DMOX reactions in the Al/Al₂O₃ system, it is more marked with sodium, because the latter has a greater effect on the wettability of alumina by aluminium.