Creep mechanisms and microstructure evolution of Nextel™ 610 fiber in air and steam

Creep rates of Nextel™ 610 alumina fibers were measured at 1100 °C and 100–500 MPa in air and steam. Steam increased creep rates and reduced fiber lifetimes. Fiber microstructures were characterized by TEM. The small amounts of grain growth, fiber-axis grain elongation, and pore growth that occur during creep were quantified. To separate the effects of stress and temperature on microstructural evolution, grain growth and elongation were also quantified for fibers heat-treated for 1–100 h in air at 1100–1500 °C. Grain growth laws were determined. The contributions of pore growth and grain elongation to creep strain were quantified. Grain elongation accounts for a large fraction of the strain during creep in air, but little in steam. Pore growth was more pronounced in steam, but does not create significant creep strain. Creep and failure mechanisms consistent with the observed microstructural changes are discussed.     

Mechanical properties of Hi-Nicalon fiber-reinforced celsian composites after high-temperature exposures in air

BN/SiC-coated Hi-Nicalon fiber-reinforced celsian matrix composites (CMCs) were annealed for 100 h in air at various temperatures to 1200 °C, followed by flexural strength measurements at room temperature. Values of yield stress and strain, ultimate strength, and composite modulus remain almost unchanged for samples annealed up to 1100 °C. A thin porous layer formed on the surface of the 1100 °C annealed sample and its density decreased from 3.09 to 2.90 g/cm³. The specimen annealed at 1200 °C gained 0.43% weight, was severely deformed, and was covered with a porous layer of thick shiny glaze which could be easily peeled off. Some gas bubbles were also present on the surface. This surface layer consisted of elongated crystals of monoclinic celsian and some amorphous phase(s). The fibers in this surface ply of the CMC had broken into small pieces. The fiber–matrix interface strength was characterized through fiber push-in technique. Values of debond stress, σ_d, and frictional sliding stress, τ_f, for the as-fabricated CMC were 0.31 ± 0.14 GPa and 10.4 ± 3.1 MPa, respectively. These values compared with 0.53 ± 0.47 GPa and 8.33 ± 1.72 MPa for the fibers in the interior of the 1200 °C annealed sample, indicating hardly any change in fiber–matrix interface strength. The effects of thermal aging on microstructure were investigated using scanning electron microscopy. Only the surface ply of the 1200 °C annealed specimens had degraded from oxidation whereas the bulk interior part of the CMC was unaffected. A mechanism is proposed explaining the various steps involved during the degradation of the CMC on annealing in air at 1200 °C.     

Interface controlled micro- and macro- mechanical properties of aluminosilicate fiber reinforced SiC matrix composites

Novel Nextel™ 440 aluminosilicate fiber reinforced SiC matrix composites, with/without chemical vapor deposited carbon interphase were fabricated by polymer derived ceramic process, and they were studied by a combination of micro- and macro- mechanical techniques such as nanoindentation, micropillar splitting, fiber push-in, digital image correction and high temperature three point bend tests. Specifically, micropillar splitting test was firstly employed to measure in-situ the localized fracture toughness. The results revealed that the carbon interphase can effectively hinder the interfacial reactions between Nextel™ 440 fiber and SiC matrix, thus remarkably weakening the composite interfacial shear strength from ∼293 MPa to ∼42 MPa, and enhance the composite fracture toughness from ∼1.8 MPa√m to ∼6.3 MPa√m, respectively. This is mainly a consequence of weak interface that triggers crack deflection at the fiber/interphase interface. Finally, this novel composite showed stable mechanical properties in vacuum at temperature range from 25 °C to 1000 °C.     

Thermal behaviour of a series of poly[B-(methylamino)borazine] for the preparation of boron nitride fibers

The thermal behaviour of a series of poly[B-(methylamino)borazine] prepared at various temperatures ranging from 140 to 200 °C is studied in the present paper as potential BN fiber precursors. It was shown that the softening capability of poly[B-(methylamino)borazine] can be tailored by controlling the temperature at which polymers were prepared to achieve melt-spinning and produce high quality green fibers. Thus as-spun fibers could be next converted into boron nitride fibers using ammonia (25–1000 °C) and nitrogen (25–1800 °C) atmospheres. The quality of boron nitride fibers was shown to depend on the first part of the pyrolysis step (25 and 1000 °C; ammonia atmosphere) in which the great majority of the weight loss necessary for boron nitride production occurs. Ideal poly[B-(methylamino)borazine] as BN fiber precursors are those prepared between 170 and 180 °C. They display appropriate melt-spinnability and ceramic conversion capability.     

Microwave-absorption properties of SiOC ceramics derived from novel hyperbranched ferrocene-containing polysiloxane

In this contribution, we design a novel strategy to synthesize SiOC ceramics by pyrolysis of hyperbranched ferrocene-containing polysiloxane (HBPSO-VF) which are synthesized by the reaction of polysiloxane (PSO) with 1,1′-Bis(dimethylvinylsilyl)ferrocene (VF). This SiOC ceramics show much lower crystallization temperature because of the capability of HBPSO-VF to incorporate metallic iron into the backbone of PSO. The usage of HBPSO-VF offers enhanced ceramic yield of 83 wt% at 1200 °C due to the deep cross-linking of hydrosilylation. Nano-sized SiC and turbostratic carbons are separated from amorphous SiOC phase when it is annealed at 1100 °C, while crystallization temperature is 1400 °C when PSO is used as polymer precursors. The minimum reflection coefficient (RC_min) of this nanocrystal-containing ceramic reaches −46 dB, exhibiting a promising prospect as a kind of electromagnetic wave (EMW) absorbing materials. This method also can be further extended to develop other functional Si-based polymer derived ceramic (PDC) systems for EMW absorption and shielding applications.     

Tensile creep behavior of three-dimensional four-step braided SiC/SiC composite at elevated temperature

This article presents experimental results for tensile creep deformation and rupture behavior of three-dimensional four-step braided SiC/SiC composites at 1100 °C and 1300 °C in air. The creep behavior at 1300 °C exhibited a long transient creep regime and the creep rate decreased continuously with time. The creep behavior at 1100 °C exhibited an apparent steady-rate regime and the creep deformation was smaller than that at 1300 °C. However, the creep rupture time at both temperatures showed little difference. The mechanisms controlling creep deformation and rupture behavior were analyzed.     

Improvement of high-temperature mechanical properties of heat treated Cf/geopolymer composites by Sol-SiO2 impregnation

Unidirectional carbon fiber reinforced geopolymer composite was prepared by ultrasonic-assisted slurry infiltration method and heat treated at 1100 °C. Then it was impregnated with Sol-SiO₂ to seal the cracks and pores formed during heat treatment. The ambient strength of composite after impregnation was enhanced by 35.6% due to the increase relative density from the starting 79% to 93.6%. Composites both before and after impregnation fractured in a non-brittle manner at both ambient and high temperatures. Over an elevated temperature range from 700 to 900 °C, the strength of the two composites showed anomalous gains and reached their maximum values at 900 °C, 322.1 and 425.1 MPa, respectively. These values were 19.8% and 16.8% higher than their ambient ones. When the temperature was further increased to 1100 °C, the impregnated composite showed superior high-temperature properties, which was attributed to the improved fiber integrity due to the Sol-SiO₂ sealing effect.     

Effects of 1600 °C annealing atmosphere on the microstructures and mechanical properties of C/SiC composites fabricated by precursor infiltration and pyrolysis

Effects of 1600 °C annealing atmosphere on microstructures and mechanical properties of the C/SiC composites fabricated by PIP route were remarkable. Due to carbothermic reductions, the ratios of weight loss of the C/SiC composites were all above 7 wt% in 1 h. Consequently, the mechanical properties all had a significant drop during the first hour of annealing because of the bonding between the fibers and matrix remarkably weaken by cracks and pores. And then the flexural strengths gradually decreased with the annealing time increasing, when the flexural moduli slightly changed within the range of 44.2–49.7 GPa. However, the fracture behaviors of the C/SiC composites annealed under Ar faster became brittle than the C/SiC composites annealed under vacuum. The C/SiC composites annealed under Ar for 5 h and under vacuum for 10 h both became brittle mainly due to the sensitive to annealing of the weak carbon interphase, while the C/SiC composites annealed under Ar for 7 h became brittle mainly due to the chemical bonding between the fibers and matrix. And these phenomena were confirmed by the post densification and the stress-releasing annealing.     

Alumina fiber-reinforced silica matrix composites with improved mechanical properties prepared by a novel DCC-HVCI method

A novel direct coagulation casting via controlled release of high valence counter ions (DCC-HVCI) method was applied to prepare the alumina fiber-reinforced silica matrix composites with improved mechanical properties. In this method, the silica suspension could be rapidly coagulated via controlled release of calcium ions from calcium iodate and pH shift by hydrolysis of glycerol diacetate (GDA) at an elevated temperature. The influence of tetramethylammonium hydroxide (TMAOH) dispersant amount, volume fraction and calcium iodate concentration on the rheological properties of suspensions was investigated. Additionally, the effect of alumina fiber contents on the mechanical properties of alumina fiber-reinforced silica matrix composites was studied systematically. It was found that the stable suspension of 50 vol% solid loading could be prepared by adding 2.5 wt% TMAOH at room temperature. The addition of 0–15 wt% alumina fibers had no obvious effect on the viscosity of the silica suspension. The controlled coagulation of the suspension could be achieved by adding 6.5 g L⁻¹ calcium iodate and 1.0 wt% GDA after treating at 70 °C for 30 min. Compressive strength of green bodies with homogeneous microstructure was in the range of 2.1–3.1 MPa. Due to the fiber pull-out and fracture behaviors, the mechanical properties of alumina fiber-reinforced composites improved remarkably. The flexural strength of the composite with 10 wt% alumina fibers sintered at 1350 °C was about 7 times of that without fibers. The results indicate that this approach could provide a promising route to prepare complex-shaped fiber-reinforced ceramic matrix composites with uniform microstructure and high mechanical properties.     

Synthesis of SiC ceramics from processed cellulosic bio-precursor

Synthesis of SiC ceramic from processed cellulosic bio-precursor was investigated. Bamboo (Bambusa tulda Roxb.) plants abundantly available in the Jorhat district of Assam, India, were selected for extraction of fibers following Kraft pulping method and bleached bamboo pulp fibers were suitably cast in the form of rectangular boards. Coir fibers available in the Alleppy district of Kerala, India, were initially digested with dilute alkali, mixed with cellulose acetate solution, air dried and then hot-pressed at 140 ± 5 °C under 2.0–2.5 MPa pressure to make rectangular boards. Well-characterized processed bio-precursors were pyrolysed at ～800 °C under flowing N₂ atmosphere to prepare the bio-carbonaceous preforms (carbon templates) which showed nearly uniform shrinkages in all directions. Coir fiber composite board carbon showed lower pyrolytic weight loss (～66%), higher density (0.49 g cm^?3), lower porosity (～58%) and narrower pore diameter (10 μm) compared to the cast bamboo pulp fiber board carbon. The carbon samples showed perfect retention of fibrous morphological features of hierarchically grown bio-structures. Ceramization of carbon templates could be done by reactive melt silicon infiltration into porous channels at ～1600 °C under vacuum. The final ceramics were adequately dense (%theoretical density > 99%), showed negligible linear dimensional changes (indicating net-dimension formation capability), presence of crystalline Si and SiC phases and duplex microstructure with complete preservation of fibrous architecture of plant bio-structure. The Si/SiC ceramic composite synthesized from coir fiber board gave room temperature 3-point flexural strength and Young's modulus values of 121 MPa and 276 GPa, respectively. Both the ceramic composites showed adequate oxidation resistance during heating at 1300 °C for 7 h in air.     

Sintering behaviour and properties of magnesium orthosilicate-hydroxyapatite ceramic

The effect of pressureless sintering on the properties of magnesium orthosilicate-hydroxyapatite (MO-HA) ceramic has been studied. The amount of MO composition in the green body was varied from 10 wt% to 50 wt% through mechanical ball milling and was subsequently sintered at varying temperatures in air atmosphere from 1000 °C to 1300 °C for 2 h. The magnesium orthosilicate phase was stable during sintering but the hydroxyapatite phase decomposed to tricalcium phosphate. The MO-HA composites generally exhibited lower mechanical properties across all the investigated composition. Nevertheless, a high fracture toughness of 2.5 MPam^1/2 was recorded for sintered body that contained 20 wt% MO. This finding indicates the potential of this ceramic composite to be used for biomedical applications.     

Influence of the carbonization temperature on the mechanical properties of thermoplastic polymer derived C/C-SiC composites

Carbon/Carbon (C/C) composites derived from the thermoplastic polymer polyetherimide (PEI) were pyrolized up to 1000 °C, subsequently carbonized in inert atmosphere up to 2200 °C and afterwards infiltrated with liquid silicon. The investigation of fibers and matrix with Raman microspectroscopy revealed, that an increased carbonization temperature leads to an increased carbon order as well as an incipient stress-induced graphitization of the carbon matrix close to the fiber surfaces at 2200 °C. The derived C/C-SiC samples show a maximum flexural strength of 180 MPa with C/C composites treated at 2000 °C and monotonically increasing Young’s moduli ranging from 49 GPa with C/C preforms treated at 1600 °C up to 59 GPa after carbonization at 2200 °C. The carbon fiber strength was evaluated with a single fiber tensile test, which showed a monotonically increased Young’s modulus and a decrease of the strength after carbonization at 2200 °C.     

Effect of sintering temperature on the characteristics of ceramic hollow spheres produced by sacrificial template technique

Ceramic hollow spheres were produced by a sacrificial template technique with subsequent sintering under temperatures ranging from 1100 °C to 1250 °C. The effect of the sintering temperature on the structure of the ceramic hollow spheres was investigated by optical and scanning electron microscopy, and a gas adsorption method. The results show that the structure of the ceramic hollow spheres can be controlled, with the retention of the hollow spherical shape, by variation of the sintering temperature. Increase of the sintering temperature from 1100 °C to 1250 °C decreased the outer diameter of the ceramic hollow spheres by 14 percent, the shell thickness by 18 percent, and the void area ratio of the shell surface by 9.2 times; both of the specific surface area and the total pore volume of ceramic hollow spheres decreased by 60 percent.     

Dynamic oxidation and protection of the PAN pre-oxidized fiber C/C composites

Pre-oxidized fibers as reinforcement are candidates for reducing the overall cost of C/C composites with superior properties. This study investigated the dynamic oxidation and protection of the pre-oxidized fiber C/C composites (Pr-Ox-C-C). According to the Arrhenius equation, the oxidation kinetics of the Pr-Ox-C-C consisted of two different oxidation mechanism with the transition point was at about 700 °C. Scanning electron microscopy investigation showed that oxidation initiated from the fiber/matrix interface of composites, whereas the matrix carbon was easily oxidized. To improve the anti-oxidant properties of Pr-Ox-C-C, a ceramic powder-modified organic silicone resin/ZrB₂-SiC coating was prepared by the slurry method. The coated samples were subjected to isothermal oxidation for 320 h at 700 °C, 800 °C, 900 °C, 1000 °C and 1100 °C with incurred weight losses of ? 1.6%, 0.77%, ? 1.28%, 0.68% and 1.19%, respectively. After 110 cycles of thermal shock between 1100 °C and room temperature, a weight loss of 1.30% was obtained. The Arrhenius curve presented four different phases and mechanisms for coating oxidation kinetics. The excellent oxidation resistance properties of the prepared coating could be attributed to the inner layer which was able to form B₂O₃-Cr₂O₃-SiO₂ glass to cure cracks, and the ZrB₂-SiC outer layer that could provide protective oxides to reduce oxygen infiltration and to seal bubbles.     

On the mechanical,thermophysical and dielectric properties of Nextel™ 440 fiber reinforced nitride matrix (N440/Nitride) composites

The Nextel? 440 fiber reinforced nitride matrix (N440/Nitride) composites were fabricated by precursor infiltration and pyrolysis (PIP) route. The results demonstrated that the original N440 fiber had a phase composition of amorphous SiO₂ and γ-Al₂O₃. Its single filament tensile strength was 3.03 GPa (at room temperature), while it dropped to 72.6% and 35.1% at 1200 °C and 1400 °C, respectively. The phase content of N440/Ntride composites was mainly γ-Al₂O₃ and amorphous BN, as well as mullite phase (formed at > 1100 °C). The composites owned a flexural strength up to 76.0 MPa at room temperature. The stair-stepping decrease in the load-displacement curve and fiber pull-outs in the fracture surface indicated a good fiber/matrix interface and toughness. By heating at 1400 °C, the composites still possessed 67.4% of original bending strength. It was found that the high temperatures caused strong fiber-matrix bonding and severe fiber degradation. The specific heat, CTE and thermal conductivity of the composites were 0.325–0.586 J g^?1 K^?1, (3.2–4.0) × 10^?6 K^?1 and 0.78–3.47 W m^?1 K^?1, respectively. The composites possessed a dielectric constant of 4.25–4.35 and loss tangent of 0.004–0.01 at 8–12 GHz. The good overall performances enabled the N440/Nitride composites advanced high-temperature wave-transparent applications.     

Microwave dielectric properties of Pb2MoO5 ceramic with ultra-low sintering temperature

Ultra-low firing microwave dielectric ceramic Pb₂MoO₅ with monoclinic structure was prepared via a conventional solid state reaction method. The sintering temperature ranged from 530 °C to 650 °C. The relative densities of the ceramic samples were about 97% when the sintering temperature was greater than 570 °C. The best microwave dielectric properties were obtained in the ceramic sintered at 610 °C for 2 h with a permittivity ∼19.1, a Q × f value about 21,960 GHz (at 7.461 GHz) and a temperature coefficient value of −60 ppm/°C. From the X-ray diffraction, backscattered electron image results of the co-fired samples with 30 wt% silver and aluminum additive, the Pb₂MoO₅ ceramics were found not to react with Ag and Al at 610 °C for 4 h. The microwave dielectric properties and ultra-low sintering temperature of Pb₂MoO₅ ceramic make it a promising candidate for low temperature co-fired ceramic applications.     

Mechanical and physical behaviors of short pitch-based carbon fiber-reinforced HfB2–SiC matrix composites

Short Pitch-based carbon fiber-reinforced HfB₂ matrix composites containing 20 vol% SiC, with fiber volume fractions in the range of 20–50%, were manufactured by hot-press process. Highly dense composite compacts were obtained at 2100 °C and 20 MPa for 60 min. The flexural strength of the composites was measured at room temperature and 1600 °C. The fracture toughness, thermal and electrical conductivities of the composites were evaluated at room temperature. The effects of fiber volume fractions on these properties were assessed. The flexural strength of the composites depended on the fiber volume fraction. In addition, the flexural strength was significantly greater at 1600 °C than at room temperature. The fracture toughness was improved due to the incorporation of fibers. The thermal and electrical conductivities decreased with the increase of fiber volume fraction, however.     

Thermal conversion of carbon fibres/polysiloxane composites to carbon fibres/ceramic composites

The aim of this work is to investigate the thermal conversion of carbon fibres/polysiloxane composites to carbon fibres/ceramic composites. The conversion mechanism of four different resins to the ceramic phase in the presence of carbon fibres is investigated. The experiments were conducted in three temperature ranges, corresponding to composite manufacturing stages, namely up to 160 °C, 1000 °C and finally 1700 °C.The study reveals that the thermal conversion mechanism of pure resins in the presence of carbon fibres is similar to that without fibres up to 1000 °C. Above 1000 °C thermal decomposition occurs in both solid (composite matrix) and gas phases, and the presence of carbon fibres in resin matrix produces higher mass losses and higher porosity of the resulting composite samples in comparison to ceramic residue obtained from pure resin samples. XRD analysis shows that at temperature of 1700 °C composite matrices contain nanosized silicon carbide. SEM and EDS analyses indicate that due to the secondary decomposition of gaseous compounds released during pyrolysis a silicon carbide protective layer is created on the fibre surface and fibre–matrix interface. Moreover, nanosized silicon carbide filaments crystallize in composite pores.Owing to the presence of the protective silicon carbide layer created from the gas phase on the fibre–matrix interface, highly porous C/SiC composites show significantly high oxidation resistance.     

Effects of sintering temperature on mechanical properties of 3D mullite fiber (ALF FB3) reinforced mullite composites

A new method to weaken the interfacial bonding and increase the strength of 3D mullite fiber reinforced mullite matrix (Mu_f/Mu) composites is proposed and tested in this paper. Firstly, Mu_f/Mu composites were fabricated through sol–gel process with varied sintering temperature. Then, the effects of sintering temperature on mechanical properties of the composites were tested. As sintering temperature was raised from 1000 °C to 1300 °C, the three-point flexural strength of the composites firstly decreased from 66.17 MPa to 41.83 MPa, and then increased to 63.17 MPa. In order to explain the relationship between composite strength and sintering temperature, morphology and structure of the mullite fibers and mullite matrix after the same heat-treatment as in the fabrication conditions of the composites were also investigated. Finally, it is concluded that this strength variation results from the combined effects of matrix densification, interfacial bonding and fiber degradation under different sintering temperatures.     

Improvement in sinterability and phase stability of hydroxyapatite and partially stabilized zirconia composites

Composites of hydroxyapatite with partially stabilized zirconia with MgO or MgF₂ were pressureless sintered between 1000 °C and 1300 °C. The reactions and transformations of phases were verified by X-ray diffraction. For the hydroxyapatite and zirconia composites with MgO, calcium from the hydroxyapatite diffused into the zirconia phase, and the hydroxyapatite decomposed to tri-calcium phosphate at sintering temperatures higher than 1000 °C. Above about 1200 °C, CaZrO₃ was formed. Composites containing the MgF₂ decomposed slower than the composites with MgO, which was verified by the changes in the lattice volume of the hydroxyapatite left in these composites. Fluorine ions in MgF₂ diffused into hydroxyapatite, which resulted in thermal stability at high sintering temperatures. Composites with MgF₂ had higher hardness than those with MgO. The lowest porosity was found in a composite initially containing 10 wt% partially stabilized zirconia and 5 wt% MgF₂.