Effect of silicon/graphite ratio and temperature on oxidation protective properties of SiC/ZrB2–SiC coatings prepared by pack cementation

To investigate the silicon/graphite ratio and temperature on preparation and properties of ZrB₂–SiC coatings, ZrB₂, silicon, and graphite powders were used as pack powders to prepare ZrB₂–SiC coatings on SiC coated graphite samples at different temperatures by pack cementation method. The composition, microstructure, thermal shock, and oxidation resistance of these coatings were characterized and assessed. High silicon/graphite ratio (in this case, 2) did not guarantee higher coating density, instead could be harmful to coating formation and led to the lump of pack powders, especially at temperatures of 2100 and 2200 °C. But residual silicon in the coating is beneficial for high density and oxidation protection ability. The SiC/ZrB₂–SiC (ZS50-2) coating prepared at 2000 °C showed excellent oxidation protective ability, owing to the residual silicon in the coating and dense coating structure. The weight loss of ZS50-2 after 15 thermal shocks between 1500 °C and room temperature, and oxidation for 19 h at 1500 °C are 6.5% and 2.9%, respectively.     

Characterization of carbon fiber-reinforced ultra-high temperature ceramic matrix composites fabricated via Zr-Ti alloy melt infiltration

Carbon fiber-reinforced ultra-high temperature ceramic matrix composites (C/UHTCMCs) were fabricated via Zr-Ti alloy melt infiltration (Zr-Ti MI) using carbon-carbon composite (C/C) preforms and alloys with three different compositions. Alloys were successfully infiltrated into C/C to form solid solutions of TiC and ZrC, with melting temperatures > 2900 °C. Notably, residual alloys were not observed after MI occurred at 1750 °C. Bending strength and fracture toughness of the C/UHTCMCs at room temperature and 1500 °C in air/Ar revealed that mechanical properties of the composites were similar to those of the C/C preform. During arc wind tunnel tests at 2000 °C, a recession of C/UHTCMCs fabricated using Ti-rich alloys was observed; however, this behavior was not observed for the composites prepared using Zr-rich alloys owing to the formation of a ZrO₂ solid solution. Accordingly, Zr-Ti MI is a viable method for preparing C/UHTCMCs without degrading the mechanical properties of the C/C preform, while increasing the ablation resistance.     

Processing and impact behavior of Al/SiCp composites fabricated by the pressureless melt infiltration method

In the current investigation, pressureless melt infiltration was applied to fabricate the Al/SiC composites based on the SiC porous preforms. The process was conducted by introducing the aluminum melt into the SiC preforms at 950 °C under the nitrogen atmosphere, without the aid of pressure. To explore development of melt infiltration, initial preforms were produced with variable SiC fractions (40, 50, and 60 vol.%) using three different SiC powders with the mean particle size of 20, 50, and 90 μm. While the infiltration of aluminum melt into the preforms with 40 vol.% initial SiC volume fraction (SiC particle size of 90 μm) resulted to the composites with final density of 0.94 theoretical density (TD), this value drops down to ～0.9 TD for the composites produced by preforms with the SiC (90 μm) volume fraction of 60 vol.%. On the other hand, composites fabricated by 50 μm SiC powder (SiC volume fraction of 40 vol.%) demonstrated the final density of ～0.91 TD. The impact resistance tests performed on the composites demonstrated an enhancement in the value of impact energy with an increase of SiC powder particle size. Results, additionally, revealed a significant superiority of impact energy for the composites fabricated by a combined melt infiltration and sintering (MIS) procedure compared to those produced by infiltration at 950 and 1350 °C.     

Microstructure and ablation behaviors of a novel gradient C/C-ZrC-SiC composite fabricated by an improved reactive melt infiltration

An improved reactive melt infiltration (RMI) route using Zr, Si tablet as infiltrant was developed in order to obtain high-performance and low-cost C/C-ZrC-SiC composite with well defined structure. Two other RMI routes using Zr, Si mixed powders and alloy were also performed for comparison. Effects of different infiltration routes on the microstructure and ablation behavior were investigated. Results showed that C/C-ZrC-SiC composite prepared by Zr, Si tablets developed a dense gradient microstructure that content of ZrC ceramic increased gradually along the infiltration direction, while that of SiC ceramic decreased. Composites prepared by Zr, Si mixed powders and alloy showed a homogeneous microstructure containing more SiC ceramic. In addition, two interface patterns were observed at the carbon/ceramic interfaces: continuous SiC layer and ZrC, SiC mixed layers. It should be due to the arising of stable Si molten pool in the tablet. Among all as-prepared samples, after exposing to the oxyacetylene flame for 60 s at 2500 °C, C/C-ZrC-SiC composite infiltrated by Zr, Si tablet exhibited the best ablation property owing to its unique gradient structure.     

Ti3Si(Al)C2-based ceramics fabricated by reactive melt infiltration with Al70Si30 alloy

Dense Ti₃Si(Al)C₂-based ceramics were synthesized using reactive melt infiltration (RMI) of Al₇₀Si₃₀ alloy into the porous TiC preforms. The effects of the infiltration temperature on the microstructure and mechanical properties of the synthesized composites were investigated. All the composites infiltrated at different temperatures were composed of Ti₃Si(Al)C₂, TiC, SiC, Ti(Al, Si)₃ and Al. With the increase of infiltration temperature from 1050 °C to 1500 °C, the Ti₃Si(Al)C₂ content increased to 52 vol.% and the TiC content decreased to 15 vol.%, and the Vickers hardness, flexural strength and fracture toughness of Ti₃Si(Al)C₂-based composite reached to 9.95 GPa, 328 MPa and 4.8 MPa m^1/2, respectively.     

Silicon carbide-based foams derived from foamed SiC-filled phenolic resin by reactive infiltration of silicon

Macro-cellular porous silicon carbide-based foams were fabricated by reactive infiltration of melt silicon into porous carbonaceous preforms pyrolyzed from foamed SiC-filled phenolic resins (PF). The SiC-filled PF foams were prepared at 80 °C with different heating rate. The effect of heating rate on the foaming behavior of the liquid SiC-filled PF mixture and the microstructure of the foams were investigated. The foamed SiC-filled PF was then pyrolyzed at 1000 °C and infiltrated by melt Si at 1600 °C, leading to the formation of open macro-cellular structure. At a heating rate of 6 °C min⁻¹, Si-infiltrated foams with a porosity of ~72% and a mean pore size of ~0.5 mm were obtained. The Si-infiltrated foams with dense struts mainly inherited the pore structure of pyrolyzed preforms. The main phases of SiC-based foams were α-SiC, β-SiC and the remnant Si, which contributed to high compressive strength of the SiC-based foams.     

Fabrication and characterization of PIP based C/SiC composites having improved mechanical properties using high modulus M40J carbon fiber as reinforcement

PIP based C/SiC composites are fabricated using high modulus M40J carbon fiber. High ceramic yield polycarbosilane (PCS) was also synthesized in the laboratory and the same was used to infiltrate the fibrous preforms. The infiltrated preforms were pyrolyzed at three different temperatures viz. 1400, 1500 and 1600 °C and termed as set-1, set-2 and set-3. Flexural strength was determined using 3-point bend fixture and the data obtained are analyzed using Weibull distribution. Average flexural strengths were found to be 691±23 MPa, 654.6±24 MPa, and 504±31 MPa for the sets 1, 2 and 3 respectively and the corresponding Weibull moduli were found to be 27.9, 25.5 and 15.6. The composites pyrolyzed at 1400 and 1500 °C, have been found to exhibit extensive fiber pull-out and thus demonstrated pseudo-ductile fracture behavior. A relatively brittle fracture was observed for the composites pyrolyzed at 1600 °C. Area under the flexural stress and displacement curve is found to be in the ratio 1.0:0.92:0.8 for the for the sets 1, 2 and 3 respectively. The effect of the pyrolysis temperature on the mechanical properties is discussed in the light of the microstructure of the composites.     

Physical properties of graphite/aluminium composites produced by gas pressure infiltration method

Graphite/aluminium composites have been produced by means of gas pressure infiltration method. Two porous graphite preforms with a porosity of 10 and 13 vol%, respectively, have been infiltrated using either a commercially 99.85 pure aluminium or an AlSi7Mg alloy. Thermal expansion coefficient, electrical conductivity and flexural strength have been determined as a function of graphite preforms and metal matrices. To investigate the susceptibility of this composite system to thermal damage, specimens were thermally cycled between 60 and 300 °C up to 1020 cycles. Infiltrated graphites exhibited a significantly higher electrical conductivity (0.34-0.51 m/Ω mm²) compared to porous graphite preforms depending on graphite type and metal matrix. Thermal cycling did not influence electrical conductivity. The coefficients of thermal expansion of the composites were at least three times lower than for monolithic aluminium. Thermal cycling has reduced these values even more, most likely due to stress relaxation processes. The infiltration of porous graphite preforms with AlSi7Mg alloy or Al99.85 has increased the flexural strength of the composites resulting in values up to 105 MPa. The decrease in mechanical strength due to thermal cycling was about 10%.     

Reactive infiltration processing of SiC/Fe–Si composites using preforms made of coked rice husks and SiC powder

A reactive infiltration processing of SiC/Fe–Si composites using preforms made of coked rice husks (RHs) and SiC powder in different ratios is reported, in which FeSi₂ alloy was used as infiltrant. The preforms were heat-treated at 1550 °C for 6 h prior to the infiltration. The coked RHs, which are composed of SiO₂ and C, were converted to SiC and poorly crystallized C by carbothermal reduction during the heat treatment. The study of the microstructure and mechanical properties of the composites shows that molten Fe–Si alloy had good wetting of the heat-treated preforms and adequate infiltration properties. Free carbon in the preform reacted with Si in the molten FeSi₂ during infiltration forming new SiC, the composition of the intermetallic liquid being moved towards that of FeSi. As a result, the infiltrated composites are composed of SiC, FeSi₂ and FeSi phases. Vickers hardness, elastic modulus, three-point flexural strength and indentation fracture toughness of the composites are found to increase with SiC additions up to 30% w/w in the preforms, reaching the values of 18.2 GPa, 290 GPa, 213 MPa and 4.9 MPa m^1/2, respectively. With the SiC addition further raised to 45% w/w, the elastic modulus, flexural strength and fracture toughness of the composite turned down probably due to high residual stress and hence the more intense induction of microcracks in the composite. De-bonding of SiC particles pulled out of the Fe–Si matrix, transgranular fracture of part of the SiC particles and in the Fe–Si matrix, and crack bridging all exist in the fracture process of the composites.     

Effect of excess silicon content on the formation of nano-layered Ti3SiC2 ceramic via infiltration of TiC preforms

The aim of this work was to investigate the effect of silicon content on the formation and morphology of Ti₃SiC₂ based composite via infiltration of porous TiC preforms. The gelcasting process was used for fabrication of preforms. It was found that the infiltrated sample at 1500 °C for 90 min from a mixture of 3TiC/1.5Si containing 92 wt.% Ti₃SiC₂. With the increasing of TiC and SiC impurity phases, Vickers hardness was increased to the maximum value of 12.9 GPa in Ti₃SiC₂–39 wt.%TiC composite. Microscopic observations showed that the Ti₃SiC₂ matrix was composed of columnar, platelike and equiaxial grains with respect to silicon content.     

On the effects of particle size and preform porosity on the mechanical properties of reaction-bonded boron carbide infiltrated with Al-Si alloy at 950 °C

The infiltration of boron carbide preforms with Al alloys at relatively low temperature prevents the formation of the undesired Al₄C₃ phase. In the present study the effect of boron carbide powder particle size on the mechanical properties and phase composition of composites infiltrated with Al-20%Si alloys at 950 °C was investigated. According to XRD analysis, the infiltrated composites contain Al₈C₇B₄, AlB₂ and AlB₁₂, as well as non-reacted Al and Si that originated from solidification of Al-Si alloy. The presence of small amounts of SiC was noted in specimens fabricated from fine boron carbide powder. No evidence for the formation of non-desired aluminum carbide phase was obtained. Infiltration of ceramic preforms with virtually the same green density generated composites with an elastic modulus and bending strength that continuously decreased from 270 GPa and 405 MPa to 195 GPa and 345 MPa for powder with 90% particles close to 3 μm and powder with 90% particles close to 180 μm, respectively. These results ambiguously confirm that boron carbide particle size strongly affects mechanical properties of reaction-bonded composites infiltrated with Al-Si alloy at 950 °C and reflect the amount of newly formed ceramic phases appearing during infiltration and the presence of defects at the metal-ceramic interface.     

Strengthening the thermal Negative Poisson's ratio structures by SiC chemical vapor infiltration

Negative Poisson's ratio structures exhibit adjustable thermal expansion behavior as the thermal stress can be dispersed or offset by torsion, bending, and tension of the struts. However, the structural stability under cyclic thermal stress significantly determines the long-term durability. Strengthening the Negative Poisson's ratio structure can ensure high thermal and mechanical reliability. The work designed a heat-induced torsional Negative Poisson's ratio structures and fabricated it by 3D printing. For efficient strengthening, the preforms were further densified by chemical vapor infiltration (CVI) of SiC to enhance the reliability. Pores and gaps in the preforms were homogeneously covered and filled by the SiC, enhancing the surface finish and mechanical performance. The heat induced torsion of the structures dispersed the heat flow in one single direction, reducing the thermal stress concentration. The independent thermal expansion change of the structural unit can offset or consume the heat dissipation stress, and further improve the reliability and thermal stability through the densification process. As a result, the 120° twisted structure exhibited an average coefficient of thermal expansion (CTE) of 6. 12 × 10^?6/K from room temperature (RT) to 500 °C, and the instantaneous CTE reached the minimum value of 4.01 × 10^?6/K at 125 °C. Meanwhile, the load-bearing capacity strengthened significantly, exhibiting the optimized strength of 11.31 MPa and Young's Modulus of 36.44 GPa, revealing a significant improvement than those of preforms, promising for high load-bearing and low expansion application of structure-function integrated low expansion material.     

Fabrication of tough SiCf/SiC composites by electrophoretic deposition using a fabric coated with FeO-catalyzed phenolic resin

A hybrid processing route based on vacuum infiltration, electrophoretic deposition, and hot-pressing was adopted to fabricate dense and tough SiC_f/SiC composites. The as-received Tyranno SiC fabric preform was infiltrated with phenolic resin containing 5 wt.% FeO and SiC powders followed by pyrolysis at 1700 °C for 4 h to form an interphase. Electrophoretic deposition was performed to infiltrate the SiC-based matrix into the SiC preforms. Finally, SiC green tapes were sandwiched between the SiC fabrics to control the volume fraction of the matrix. Densification close to 95% ρ_theo was achieved by incorporating 10 wt.% Al₂O₃-Sc₂O₃ sintering additive to facilitate liquid phase sintering at 1750 °C and 20 MPa for 2 h. X-ray diffraction and Raman analyses confirmed the catalytic utility of FeO by the formation of a pyrolytic carbon phase. The flexural response was explained in terms of the extensive fractography results and observed energy dissipating modes.     

Synthesis,Characterization, and Microstructure of ZrC/SiC Composite Ceramics via Liquid Precursor Conversion Method

The ceramic precursor for ZrC/SiC was prepared via solution‐based processing using polyzirconoxane, polycarbosilane, and divinylbenzene. The precursor could be transformed into ZrC/SiC ceramic powders at relative low temperature (1500°C). The cross‐linking process of precursor was studied by FT–IR. The conversion from precursor into ceramic was investigated by TGA, XRD. The ceramic compositions and microstructures were identified by element analysis, Raman spectra, SEM, and corresponding EDS. The results indicated that the ceramic samples remained amorphous below 1000°C and t–ZrO₂ initially generated at 1200°C. Further heating to 1400°C led to the formation of ZrC and SiC with the phase transformation of ZrO₂ and almost pure ZrC/SiC could be obtained upon heat‐treatment at 1500°C. During heat treatments, the ceramic sample changed from compact to porous due to carbothermal reduction. The ceramic powders with particle size of 100 nm~400 nm consisted of high crystalline degree ZrC and SiC phases, and Zr, Si, C were well distributed at the different sites in ceramic powders. The free carbon content was lowered to 1.60 wt% in final ZrC/SiC composite ceramics.     

Processing of silicon carbide–boron carbide–aluminium composites

The aim of this work was to shed light on the wetting mechanism in the SiC–B₄C–Al system and to explore processing routes that enable infiltration of Al alloys into these ceramic powder mixtures without the formation of the deleterious reaction product Al₄C₃. For this purpose, powder mixtures consisting of SiC and pre-treated B₄C were pressureless infiltrated with Al alloys at relatively low temperatures under an inert gas atmosphere. Depending on the characteristics of the starting powders fully infiltrated composites were achieved in the temperature range of 935–1420 °C. It was observed that addition of pre-treated B₄C to SiC enabled complete infiltration of the ～0.6 cm thick preforms. The bulk density of all produced composites was >98% of the X-ray density. By controlling the surface chemistry and particle size of the starting powders as well as the processing conditions, the wetting behaviour and reaction kinetics of this system could be tailored so as to render fully dense SiC–B₄C–Al composites devoid of Al₄C₃.     

Fabrication and properties of macro-porous SiC using Al2O3–Y2O3–SiO2 as bonding additives

Macro-porous SiC was fabricated without using pore-forming agents by an in situ reaction bonding process. A bonding additive, Al₂O₃–Y₂O₃–SiO₂, with a low melting temperature was mixed with SiC particles and sintered at 1500 °C and 1600 °C for 1 h in Ar. Macro-porous SiC with a porosity of 32.7–45.9%, a pore size of 3.4–4.2 μm, and a relatively narrow and uniform pore size distribution was fabricated by varying the amount of bonding additive. The flexural strength of macro-porous SiC prepared at 1500 °C increased from 47.2 MPa to 71.2 MPa while the porosity decreased from 45.9% to 42.8%, respectively. When the sintering temperature of the macro-porous SiC was increased to 1600 °C, the flexural strengths were significantly reduced to 32.6–35.6 MPa, along with a reduction in porosity and pore size. The permeability of macro-porous SiC prepared at 1500 °C varied from 1.59 × 10^?12 m² to 1.26 × 10^?12 m², depending on the porosity. As the sintering temperature increased from 1500 °C to 1600 °C, the permeability decreased to less than 1.00 × 10^?12 m² because of the reduced porosity and average pore size. The electrical resistivity of macro-porous SiC prepared at 1500 °C and 1600 °C varied from 2.7 × 10⁸ Ω-cm to 1.4 × 10⁹ Ω-cm and from 1.3 × 10⁸ Ω-cm to 1.7 × 10⁹ Ω-cm, respectively, with increasing volume percent of bonding additives. The relatively high electrical resistivity was apparently due to neck bonding phase between SiC particles formed by phases consisting of Y₂Si₂O₇, YAG, and residual Al₂O₃.     

Densification behaviour and mechanical properties of B4C–SiC intergranular/intragranular nanocomposites fabricated through spark plasma sintering assisted by mechanochemistry

High-performance B₄C–SiC nanocomposites with intergranular/intragranular structure were fabricated through spark plasma sintering assisted by mechanochemistry with B₄C, Si and graphite powders as raw materials. Given their unique densification behaviour, two sudden shrinkages in the densification curve were observed at two very narrow temperature ranges (1000–1040 °C and 1600–1700 °C). The first sudden shrinkage was attributed to the volume change in SiC resulting from disorder–order transformation of the SiC crystal structure. The other sudden shrinkage was attributed to the accelerated densification rate resulting from the disorder–order transformation of the crystal structure. The high sintering activity of the synthesised powders could be utilised sufficiently because of the high heating rate, so dense B₄C–SiC nanocomposites were obtained at 1700 °C. In addition, the combination of high heating rate and the disordered feature of the synthesised powders prompted the formation of intergranular/intragranular structure (some SiC particles were homogeneously dispersed amongst B₄C grains and some nanosized B₄C and SiC particles were embedded into B₄C grains), which could effectively improve the fracture toughness of the composites. The relative density, Vickers hardness and fracture toughness of the samples sintered at 1800 °C reached 99.2±0.4%, 35.8±0.9 GPa and 6.8±0.2 MPa m^1/2, respectively. Spark plasma sintering assisted by mechanochemistry is a superior and reasonable route for preparing B₄C–SiC composites.     

Fabrication of Cf/ZrC–SiC composites using Zr–8.8Si alloy by melt infiltration

Cf/ZrC–SiC composites were fabricated by melt infiltration at 1800 °C using Zr–8.8Si alloy and carbon felt preforms. Microstructural analysis showed the formation of both ZrC and SiC phases in the matrix, in which ZrC acted as a main composition of the resulting composites. The results showed that carbon matrix reacted preferentially with Si of Zr–8.8Si alloy, which caused the formation of SiC first and then ZrC. The designed carbon coating by pyrolysis prevented the severe reaction between fibers and the melt. The composites could be more dense and uniform with the bending strength of 53.3 MPa, when preforms had a high open porosity (47.2%) with small size pores (10–40 μm).     

Preparation and characterization of freestanding SiC(Ti,B) films derived from polycarbosilane with TiN and B as additives

Freestanding SiC(Ti, B) films with high temperature resistance were fabricated from polymer precursor of polycarbosilane (PCS) blended with 0.26 wt% TiN and 0.74 wt% B powders. Results reveal that SiC(Ti, B) films with good mechanical properties are uniform and dense. After high temperature annealing at 1500 °C in argon, SiC(Ti, B) films exhibit better high temperature resistance as compared to SiC films without additives, which implies their potential applications in ultra-high temperatures (exceeding 1500 °C) microelectromechanical systems (MEMS). Sintering additives are effective in suppressing the growth of SiC crystals and decreasing the content of oxygen and free carbon, which is normally beneficial to enhance high temperature resistance of films.     

Al2O3/Cu-O composites fabricated by pressureless infiltration of paper-derived Al2O3 porous preforms

Al₂O₃/Cu-O composites were fabricated from the paper-derived alumina matrix infiltrated with a Cu-3.2?wt% O alloy. Paper-derived alumina preforms with an open porosity ranging from ～ 14 to ～ 25?vol% were prepared by sintering of alumina-loaded preceramic papers at 1600?°C for 4?h. Pressureless infiltration at 1320?°C for 4?h of the preforms with Cu–O alloy resulted in the nearly dense materials with good mechanical and electrical properties, e.g. fracture toughness up to 6?MPa?m^0.5, four-point-bending strength up to 342?MPa, Young's modulus up to 281?GPa and electrical conductivity up to 2?MS/m depending on the volume fraction of copper alloy in the composites. The technological capability of this approach was demonstrated using prototypes in various engineering fields fabricated by lamination, corrugating and Laminated Object Manufacturing (LOM) methods.