Microstructure and properties of porous anorthite/mullite whiskers ceramics with high porosity

Porous anorthite/mullite whiskers ceramics with high porosity (>91%) and high strength (>0.45 MPa) have been successfully prepared by foam gel-casting method. Effects of extra mullite whiskers on properties including thermal conductivity and compressive strength at different temperatures were investigated and discussed in terms of microstructure observed through SEM and TEM. The results showed that the addition of extra mullite whiskers in certain content could effectively reduce thermal conductivity, improve the compressive strength both at room and high temperature at same time. When the mullite whiskers content was 20 mol%, the porosity was as high as 91.6 ± 0.19%, the thermal conductivity was low to 0.034 ± 0.003 W/(m·K), and the compressive strength at 1000°C was high to 0.64 ± 0.11 MPa three times to the pure one. Small pores, small grains, and more phase interface or grain boundary caused by the addition of extra mullite whiskers were the main factors for low thermal conductivity. Meanwhile, small pores, closely bonded small grains, and the stable three-dimension network formed by mullite whiskers helped to improve strength.     

One-step preparation of asymmetric ceramic membranes based on sea urchin-like mullite whisker skeletons and their oil-water separation properties

In this work, novel sandwich-type asymmetric ceramic microfiltration membranes with a sea urchin-like mullite whisker skeleton were prepared one step. Their structural properties and oil-water separation performance were investigated. The results show that after sintering at 1400 °C, the prepared membrane possesses good hydrophilic, underwater oleophobic, and anti-fouling properties. During the continuous separation of a 300 mg/L oil-in-water emulsion, a maximum stable flux of 267 L·m⁻²·h⁻¹ was achieved without membrane cleaning. After chemical cleaning and simple physical cleaning, the membranes recovered to a steady flux of 397 L·m⁻²·h⁻¹ and 305 L·m⁻²·h⁻¹, respectively, and maintained a 95% oil rejection. The good underwater oleophobicity and selective permeability brought about by the flat-lying whiskers on the top surface, coupled with the efficient water channels between the sea urchin-like structures inside the membrane, are considered to be the main reasons for its improved separation characteristics over conventional low-cost ceramic membranes.     

Formation of Ti3SiC2 interphase coating on SiCf/SiC composite by electrophoretic deposition

To improve the oxidation resistance of SiC composites at high temperature, the feasibility of using Ti₃SiC₂ coated via electrophoretic deposition (EPD) as a SiC fiber reinforced SiC composite interphase material was studied. Through fiber pullout, Ti₃SiC₂, due to its lamellar structure, has the possibility of improving the fracture toughness of SiC_f/SiC composites. In this study, Ti₃SiC₂ coating was produced by EPD on SiC fiber; using Ti₃SiC₂‐coated SiC fabric, SiC_f/SiC composite was fabricated by hot pressing. Platelet Ti₃SiC₂ powder pulverized into nanoparticles through high‐energy wet ball milling was uniformly coated on the SiC fiber in a direction in which the basal plane of the particles was parallel to the fiber. In a 3‐point bending test of the SiC_f/SiC composite using Ti₃SiC₂‐coated SiC fabric, the SiC_f/SiC composite exhibited brittle fracture behavior, but an abrupt slope change in the strength‐displacement curve was observed during loading due to the Ti₃SiC₂ interphase. On the fracture surface, delamination between each layer of SiC fabric was observed.     

Fibrous porous mullite ceramics modified by mullite whiskers for thermal insulation and sound absorption

In order to meet the demand for thermal insulation and sound absorption, fibrous porous mullite ceramics (FPMC) with high porosity and an interconnected pore structure were prepared, followed by a pore structure modification with in situ grown mullite whiskers on the three-dimensional framework of the FPMC. The resultant hierarchical material exhibited superior sound absorption performance in the low-to-medium frequency to most reported sound-absorbing materials, as well as a sufficient compressive strength of 1.26 MPa with low thermal conductivity of 0.117 W·m^?1·K^?1. Moreover, the effects of solid content and mullite whiskers on the microstructure and physical properties of the material were analyzed. The increase of solid content led to increased compressive strength and thermal conductivity and decreased frequency corresponding to the first sound absorption peak. The thermal conductivity and compressive strength of the material increased as the mullite whiskers grew, while the median pore size decreased.     

Effect of SiC whiskers on the anti-oxidation properties of Yb2Si2O7/mullite/SiC tri-layer environmental barrier coating for CMCs

The mullite and ytterbium disilicate (β-Yb₂Si₂O₇) powders as starting materials for the Yb₂Si₂O₇/mullite/SiC tri-layer coating are synthesized by a sol–gel method. The effect of SiC whiskers on the anti-oxidation properties of Yb₂Si₂O₇/mullite/SiC tri-layer coating for C/SiC composites in the air environment is deeply studied. Results show that the formation temperature and complete transition temperature of mullite were 800–1000 and 1300°C, respectively. Yb₂SiO₅, α-Yb₂Si₂O₇, and β-Yb₂Si₂O₇ were gradually formed between 800 and 1000°C, and Yb₂SiO₅ and α-Yb₂Si₂O₇ were completely transformed into β-Yb₂Si₂O₇ at a temperature above 1200°C. The weight loss of Yb₂Si₂O₇/(SiC_w–mullite)/SiC tri-layer coating coated specimens was 0.15 × 10⁻³ g cm⁻² after 200 h oxidation at 1400°C, which is lower than that of Yb₂Si₂O₇/mullite/SiC tri-layer coating (2.84 × 10⁻³ g cm⁻²). The SiC whiskers in mullite middle coating can not only alleviate the coefficient of thermal expansion difference between mullite middle coating and β-Yb₂Si₂O₇ outer coating, but also improve the self-healing performance of the mullite middle coating owing to the self-healing aluminosilicate glass phase formed by the reaction between SiO₂ (oxidation of SiC whiskers) and mullite particles.     

In situ Y2Si2O7 coatings on Hi-Nicalon-S SiC fibers: Phase formation and fiber strength

Y₂Si₂O₇ coatings were formed on Hi-Nicalon-S SiC fibers by reaction of solution-derived YPO₄ coatings with glass SiO₂ scales formed by fiber oxidation. Two oxidation methods were used: pre-oxidation, where fibers were oxidized prior to YPO₄ coating, or post-oxidation, where fibers were first coated with YPO₄ and then oxidized. Fibers with YPO₄/SiO₂ films were heat-treated in argon at 1200°C for 20 hours to react YPO₄ and SiO₂ to Y₂Si₂O₇. The effects of SiO₂ to YPO₄ film thicknesses on fiber strength and on the Y₂Si₂O₇formation kinetics were investigated. An optimized process to obtain single-phase continuous Y₂Si₂O₇ coatings on Hi-Nicalon-S fibers with low loss in fiber strength is suggested.     

Insights into internal oxidation of SiC/BN/SiC composites

The article presents new observations of the physical manifestations of internal oxidation and volatilization in SiC/BN/SiC composites. The observations are made on both unbroken and broken minicomposite specimens before and after 12 h exposures at 1000°C in dry air with 10 ppm water vapor. The observations are enabled by a sample preparation method involving ion-mill sectioning and polishing. Complementary analyses of volatilization and closure of resulting gaps are also presented. The observations show that BN is generally consumed in two stages: (i) through reaction with oxygen along the interfaces with both the fiber and the matrix, producing two concentric annular pockets of borosilicate glass and an intervening annulus of progressively thinning BN; and (ii) subsequent volatilization, through the reaction of boria with trace amounts of water vapor in the environment to form borohydroxide gases. The spatial extent to which these processes proceed is governed by a competition between the outward diffusion of reaction gases through both matrix cracks and interface gaps produced by boria volatilization, and the formation of oxides on the newly exposed surfaces of fibers, matrix, and coating.     

Formation of SiC whiskers/leucite-based ceramic composites from low temperature hardening geopolymer

In this study, SiC whiskers (SCWS) reinforced geopolymer composites (SCWS/KGP) and their ceramic products (SCWS/leucite) were prepared, and effects of SiC whiskers contents on the microstructure and flexural strength of the SCWS/KGP and SCWS/leucite composites were investigated. The results show that the whisker addition has little influence on both phase composition and thermal shrinkage of the KGP composites, but a suitable content of whisker will result in the improved flexural strength, and when the SCWS content is 2 wt%, flexural strength of the SCWS/KGP composite is enhanced by 95% compared with the neat geopolymer. The flexural strength of the composites can be further enhanced significantly after the composites being treated at 1100 °C and 1200 °C and flexural strength of the composite with SCWS content of 2 wt% was 107% and 125% higher than the untreated counterpart, respectively. The increase in flexural strength of the composites should be attributed to the strong leucite formation, whisker debonding and pulling out from matrix during the fracturing process based on the good interfacial bonding state between whisker and leucite matrix.     

离心场强化晶硅切割废料Si/SiC分离过程油水分相

对切割料中Si和SiC的高效分离进行了研究,利用晶硅切割废料中Si和SiC表面性质的差异,向浆料中加入柴油并充分乳化,使SiC吸附在油滴上实现Si/SiC分离,对乳化后的浆料施加离心力强化油水分相,调节浆料pH值改变颗粒表面Zeta电位,调控乳化后的油滴大小,研究了Si/SiC分离效果、分相时间与浆料pH的关系及附有SiC的油滴表观密度与油滴直径的关系,对乳化后的浆料分别施加超重力系数为10, 50, 100, 150和200的离心力,考察了离心时间2 min时的分相效果和Si/SiC分离效果。结果表明,常重力场中,油滴尺寸越小,分相时间越长,但SiC去除效果变好,pH=7时,水相SiC含量为4.23wt%。油滴直径小于64 ?m时,油滴在浆料中不可上浮。离心场中,超重力系数为100, pH=7时,水相中SiC含量为5.47wt%,分相时间由460 min缩短为2 min。通过对离心场中SiC的受力分析解析了离心场中SiC在油滴表面的赋存状态,证实离心场作用下,SiC沿油滴表面向离心力方向移动使油滴对SiC的吸附力减小。     

Fugitive Interfacial Carbon Coatings for Oxide/Oxide Composites

The effectiveness of fugitive interfacial carbon coatings in Nextel™ 720-based composites was investigated. Dense (>90%) matrix (calcium aluminosilicate, 0° and ±45°) composites and porous matrix (mullite/alumina, eight-harness satin fabric) composites were fabricated and tensile tested in two control conditions (uncoated or carbon-coated) and with the carbon removed (fugitive interface). Results indicated that carbon removal in dense matrix composites did not significantly change unidirectional composite strength, even after long-term exposure at 1000°C. For porous matrix composites, composite strength was independent of the fiber/matrix interface, even after exposure at 1150°C for 500 h in air.     

Effects of interface bonding properties on cyclic tensile behavior of unidirectional C/Si3N4 and SiC/Si3N4 composites

In this paper, the effect of fiber/matrix interface bonding properties on the cyclic loading/unloading tensile stress?strain hysteresis loops of 2 different ceramic‐matrix composites (CMCs), ie, C/Si₃N₄ and SiC/Si₃N₄, has been investigated using micromechanical approach. The relationships between the damage mechanisms (ie, matrix multicracking saturation, fiber/matrix interface debonding and fibers failure), hysteresis dissipated energy and internal frictional damage parameter have been established. The damage evolution processes under cyclic loading/unloading tensile of C/Si₃N₄ and SiC/Si₃N₄ composites corresponding to different fiber/matrix interface bonding properties have been analyzed through damage models and interface frictional damage parameter. For the C/Si₃N₄ composite with the weakest fiber/matrix interface bonding, the composite possesses the lowest tensile strength and the highest failure strain; the hysteresis dissipated energy increases at low peak stress, and the stress?strain hysteresis loops correspond to the interface partially and completely debonding. However, for the SiC/Si₃N₄ composite with weak interface bonding, the composite possesses the highest tensile strength and intermediate failure strain; and the hysteresis dissipated energy increases faster and approaches to a higher value than that of composite with the strong interface bonding.     

Mullite whisker toughened mullite coating to enhance the thermal shock resistance of SiC pre-coated carbon/carbon composites

In order to improve the thermal shock resistance of the coated carbon/carbon (C/C) composites, a mullite whisker toughened mullite coating was fabricated on the surface of SiC pre-coated C/C composites (SiC-C/C) by molten-salt method with a later hot dipping process. The phase compositions, surface and cross-section microstructures, high temperature thermal shock resistance of the as-prepared multi-layer coatings were investigated. Results show that the introduction of mullite whiskers can effectively improve the density of the mullite outer coating and decrease the cracking of the coating during the thermal shock cycle process. After 100 times thermal shock cycles between 1773 K and room temperature, only 1.87 × 10⁻³ g cm⁻² weight loss has been detected, indicating the achievement of the excellent thermal shock resistance.     

A TiO2 modified whisker mullite hollow fiber ceramic membrane for high-efficiency oil/water emulsions separation

Design and preparation of membranes with ultrahigh separation performance and antifouling property for oil-in-water (O/W) emulsions remains challenging. In this study, a high flux mullite/TiO₂ ceramic composite membrane was prepared via multi-precipitation of TiO₂ on a whisker mullite hollow fiber support synthesized by combining phase inversion and high-temperature sintering techniques. The results showed that the generated whisker mullite structure improved the permeation flux, and the micro-nano structured TiO₂ functional layer endowed the membrane surface with superhydrophility and stability. The retention of the optimal composite membrane (M20T13) that was soaked in the titanium solution 20 times for 13 min each time for the O/W emulsions like n-hexane, toluene and engine oil maintained over 98 %, and the flux after 6 h filtration was 668.34 L·m⁻²·h⁻¹, 487.25 L·m⁻²·h⁻¹ and 258.66 L·m⁻²·h⁻¹, respectively, much higher than that of the optimal substrate (F3A1, mass ratio of fly ash: Al₂O₃ = 3:1). Moreover, the flux recovery rate of M20T13 was much higher than that of F3A1 after chemical backwashing. This work manifests great potential in O/W treatment fields.     

Thin coatings of hafnon abate oxidative recession of SiC fibers

The oxidation behavior of SiC fibers coated with (a) undoped polysilazane and (b) precursors containing a mixture of polysilazane and hafnium butoxide in equal weight fractions, is reported. The coatings were prepared by repetitive cycles of nanolayer depositions, as reported in recent publications. The oxidation experiments were carried out at 1400°C in ambient air (Boulder, CO) for up to 100 hours. The extent of degradation of SiC was measured by the recession in the diameter of the fibers as a function of time. The fibers with undoped polymer precursor recessed significantly, whereas the fibers coated with HfSiCNO remained essentially unchanged. These results are in agreement with earlier work from our laboratory where the resilience of hafnon and zircon, as well as hafnia and zirconia, against high-temperature corrosion in streaming humid environments had been highlighted.     

AlPO4-coated mullite/alumina fiber reinforced reaction-bonded mullite composites

A precursor for reaction-bonded mullite (RBM) is formulated by premixing Al₂O₃, Si, mullite seeds and mixed-rare-earth-oxides (MREO). An ethanol suspension thereof is stabilized with polyethyleneimine protonated by acetic acid. The solid in the suspension is infiltrated into unidirectional mullite/alumina fiber-preforms by electrophoretic infiltration deposition to produce fiber-reinforced, RBM green bodies. Crack-free composites with ≤25% porosity were achieved after pressureless sintering at 1300 °C. Pre-coating the fibers with AlPO₄ as a weak intervening layer facilitates significant fiber pullout on composite fracture and confers superior damage tolerance. The bend strength is 170 MPa at 25 °C ≤ T ≤ 1100 °C. At 1200 °C, the composite fails in shear due to MREO-based, glassy phase formation. However, the AlPO₄ coating acts as a weak layer even after thermal aging at 1300 °C for 100 h.     

Damage evolution in SiC/SiC unidirectional composites by X-ray tomography

Melt infiltrated SiC/SiC ceramic matrix composite unidirectional (UD) composite specimens were imaged under load using X-ray microtomography techniques in order to visualize the evolution of damage accumulation and to quantify damage mechanisms within the composite such as matrix cracking and fiber breaking. The data obtained from these in situ tensile tests were used in comparison with current models and literature results. Three-dimensional (3D) tomography images were used to measure the location and spacing of matrix cracking that occurred at increasing stress increments during testing within two UD composite specimens. The number of broken fibers and the location of each fiber break gap that occurred within the volume of both specimens were also quantified. The 3D locations of fiber breaks were correlated with the location of each matrix crack within the volume of the specimen and it was found that at the stress scanned directly before failure, most of the fiber breaks occur within 100 microns of a matrix crack.     

SiC/SiC复合材料及其应用

日本开发的Nicalon和Tyranno两种品牌的SiC纤维占有世界上绝对性的市场份额。SiC/SiC复合材料典型的界面层是500 nm厚的单层热解碳(PyC)涂层或多层(PyC-SiC)n涂层,在湿度燃烧环境及中高温条件下界面层的稳定性是应用研究的重点。SiC/SiC复合材料,包括CVI-SiC基体和日本开发的Tyranno hex和NITE-SiC基体等,具有耐高温、耐氧化性和耐辐射性的特点,在航空涡轮发动机部件、航天热结构部件及核聚变反应堆炉第一壁材料等方面正开展工程研制应用。     

Nanosized (Zr,Hf)O2 coating reinforced by AlN whiskers for the ablation protection of SiC coated C/C composites

In this work, AlN whisker-reinforced (Zr, Hf)O₂ coating was prepared on SiC coated carbon/carbon composites by sol-gel and plasma spraying methods. Its cyclic ablation resistance was evaluated using an oxyacetylene torch with a heat flux of 2.38 MW/m². After ablation, the coating showed apparently decreased crack sizes and quantity as compared with the one without AlN whisker addition, pointing out its better crack tolerance. Moreover, the coating had a thinner oxidized region based on the linear ablation rate (−0.042 µm/s), greatly lower than that of pure oxide coating (−0.922 µm/s). After detailed observation and characterization, probable protection mechanism was proposed.     

Analysis of SiC/SiC composites for energy applications at ambient conditions

Plain weave planar and biaxially braided tubular SiC/SiC CMCs are evaluated in tension and four-point bending, respectively, at ambient conditions. Custom-designed fixtures for CMC testing are developed for each loading mode and are coupled with three-dimensional digital image correlation. Stereoscopic image correlation analysis reveals crack initiation and failure sites to provide insight into stress redistribution mechanisms. Scanning electron microscopy is performed postmortem to determine the influence of microstructural features on crack initiation and failure. Crack spacing is measured in situ by stereoscopic image correlation and confirmed by SEM measurements to relate to underlying tow-tow crossing points. Triangulated surface heights of plain weave tow architecture are used to determine that subtle differences in neighboring transverse tow angle, which vary within a range of ±4° from horizontal, have no significant effect on final fracture location. The results presented reaffirm the state of current SiC/SiC CMCs developed for energy applications and will help to further improve SiC/SiC and other CMCs.     

Cf/SiC复合材料的制备及性能的研究

采用料浆渗积-有机前躯体裂解工艺制备碳纤维增强碳化硅陶瓷基复合材料.制备材料的抗弯强度达283 MPa,断裂韧性达12.1 MPa·m1/2.