Effects of heating rate on the structure and properties of SiOC ceramic foams derived from silicone resin

Silicon oxycarbide ceramic foams were fabricated in a single step manufacturing process using in situ foaming of SiOC powders loaded silicone resin. The effects of heating rate on the porosity, compressive strength and microstructure of the ceramic foams were investigated. The porosity (total and open) increased firstly and then decreased with increasing heating rate. It was possible to control the total and open porosity of ceramic foams within a range of 81.9–88.2% and 62.4–72.5% respectively, by adjusting the heating rate from 0.25 °C/min to 3 °C/min while keeping the silicone resin content at 90 vol%. However, the compressive strength decreased with increasing the heating rate progressively, and the average compressive strength of the foams was in the range of 1.0–2.3 MPa. Micrographs indicated that the ceramic foams which cross-linked at a heating rate less than 1 °C/min had a well-defined open-cell and regular pore structure.     

Effect of thermal treatment on Egyptian rice straw hardboard

The effects of thermal treatment on the bending strength and water resistance of Egyptian rice straw hardboard manufactured with, or without, different amounts of resins, were investigated. The bending strength falls with increase in heating time and temperature for samples up to 1.5% resin; whereas hardboard with 3% resin showed an initial improvement in bending strength after heating at 140, 160 and 180°C. Heating samples at 200°C drastically reduces bending strength. Water resistance of all samples was improved by heat treatment.     

Efficacy of novel cleansing agent for the decontamination of lithium disilicate ceramics: a shear bond strength study

Purpose: To investigate the efficacy of Ivoclean as a ceramic cleansing agent, by assessing shear bond strength of pre-etched lithium disilicate (LD) ceramic to resin cement.

Materials and Methods: Seventy LD discs (10 × 10 × 4 mm) were fabricated and etched using 5% hydrofluoric acid (HF) for 20 s. Ten specimens were not exposed to saliva and silicone disclosing medium (negative control). The other 60 specimens, divided into six groups (n = 10), were exposed to saliva for 20 s and silicone disclosing medium for 3 min. Following contamination, 10 specimens were not cleansed (positive control). The remaining five groups were exposed to one of the five different cleansing agents: 96% isopropanol, 37% phosphoric acid-30 s, 5% HF acid- 20 s, 5% HF acid- 120 s, and Ivoclean paste-20 s. All specimens were treated with primer and bonded to a self-curing resin cement. Before shear bond strength testing, all specimens were thermocycled (3000 cycles; 5–55°).

Results: Contamination of pre-etched LD ceramic specimens significantly reduced the shear bond strength values from 22.39 ± 0.38 MPa (negative control) to 6.54 ± 0.90 MPa (positive control) (p < 0.05). Cleansing of contaminated ceramic specimens with 5% HF acid [20 s (19.28 ± 1.06 MPa) and 120 s (20.04 ± 1.09 MPa)] and Ivoclean (18.30 ± 0.97) provided significantly higher bond strength values than other cleansing methods with 37% phosphoric acid and 96% isopropanol (p < 0.05).

Conclusion: Ivoclean and 5% HF acid were found to be effective in cleansing of LD ceramic surface by demonstrating maximum increase in shear bond strength values as compared to contaminated LD ceramics.     

A heat-resistant preceramic polymer with broad working temperature range for silicon carbide joining

A room temperature curable heat-resistant adhesive with broad working temperature range was prepared through organic and inorganic modification. The preceramic polymethylsiloxane showed low bonding strength for silicon carbide from 400 °C to 600 °C because of the decomposition of polymer network. So the modification with epoxy resin was used to generate strong blending and copolymerization network which decomposed at higher temperature over 500 °C. The ceramization of active fillers and preceramic polymer compensated the bonding strength with rising temperature, thus eliminating the weak stage from 400 °C to 600 °C. The modification with fillers greatly improved its bonding strength at high temperature over 1000 °C. Consequently, the modified adhesive exhibited outstanding bonding strength tested at room temperature between 9.29 ± 0.56 MPa and 37.28 ± 1.33 MPa after heat-treatment from 25 °C to 1500 °C and the bonding strength directly tested at the temperature from 25 °C to 800 °C over 8.21 ± 0.40 MPa. The adhesive shows the potential to extend the application for engineering ceramic joining.     

Effect of synergism of solid loading and sintering temperature on microstructural evolution and mechanical properties of 60 vol% high solid loading ceramic core obtained through stereolithography 3D printing

Solid loading has a significant effect on the curing behavior of slurry and the microstructure and properties of the ceramic core. A high-solid loading slurry can effectively improve the sintering densification of ceramic particles and improve the interlayer bonding strength and mechanical properties at both 25 °C room and higher temperatures. Herein, based on the photopolymerization theory of ceramic slurry, the solid loading was increased from 45 to 60 vol% by adjusting the composition ratio of the resin ceramic powder. Additionally, the optimal sintering temperature of the 60 vol% solid loading ceramic core was 1200 °C. The synergistic effect of the solid loading and sintering temperature controls the sintering shrinkage of the sample within 3.2%; the porosity, high temperature, and room temperature flexural strength were approximately 30%, 24 MPa, and 10 MPa, respectively. The printing preparation of high-solid loading ceramic cores can be used to guide optimizing process parameters on an industrial scale.     

Effect of hybrid hollow microspheres on thermal insulation performance and mechanical properties of silicone rubber composites

Hollow microspheres (HM) of ceramic, silica, and glass‐filled silicone rubber (SR) composites were prepared, and the effects of hybrid HM on thermal and mechanical properties of composites were investigated. The results indicate that hybrid HM can effectively improve the thermal insulation property of HM/SR composites. Especially, for sample 15S, the thermal conductivity and thermal degradation temperature reached 0.1273 W/m K and 521 °C (45 °C higher than that of neat SR), respectively. Besides, thermal insulation performance was improved, showing as a temperature of 103.2 °C after 15 min heating, which is 37.8 °C lower than that of SR. The tensile strength of composites was enhanced from 1.92 MPa at 11.56 vol % hollow silica microspheres (HSM) loading to 3.08 MPa at 21.88 vol % HSM loading. Moreover, the compressive strength was improved from 3.33 to 5.68 MPa by introducing more hollow ceramic microspheres into the matrix, in this case, from 7.79 to 15.33 vol %. Furthermore, the failure mechanism was analyzed. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46025.     

Effect of self etching ceramic primer and universal adhesive on bond strength of lithium disilicate ceramic

The clinical success of ceramic restorations is affected by the ceramic bonding procedure. The objective of the study was to evaluate the effect of different surface treatments, including the use of self-etching ceramic primer (SECP), on resin cement-glass ceramic bond strength. Thirty lithium disilicate ceramic (LDC) rectangles (3 mm × 3 mm × 8 mm) were fabricated Specimens were randomly assigned into three experimental groups (n = 10) according to the surface treatment: Group 1-hydrofluoric acid [HF acid]+ silane + universal adhesive; Group 2-HF + universal adhesive; Group 3-SECP + universal adhesive. All specimens were stored in distilled water for 24 h at 37 °C and shear bond strength (SBS) was tested at a crosshead speed of 0.5 mm (Universal Testing machine-Instron). Failure modes were evaluated using a digital microscope for all specimens. Analysis of variance and the Tukey post hoc tests using SPSS (Version 22.0, IBM, New York, USA) were used to analyze data. The SBS of groups 1 (19.74 ± 1.28 MPa) and 3 (21.11 ± 2.07 MPa) were significant higher than group 2 (14.80 ± 1.94 MPa). The SBS values for specimens in groups 1 (19.74 ± 1.28 MPa) and 3 (21.11 ± 2.07 MPa) were comparable. Adhesive, mixed and cohesive failure modes were observed and mixed failure was the most common in all groups. Therefore, the use of SECP and universal adhesive is recommended as an alternative to the use of HF acid in combination with ceramic primer while bonding to LDC.     

Experimental study on mechanical properties of silica-based ceramic core for directional solidification of single crystal superalloy

The effects of holding time in Bridgman furnace on mechanical properties of injection molded silica-based ceramic cores for directional solidification of SX superalloy have been investigated. The cylindrical samples (S0) were sintered at 1000 ℃ for 60 min, and some of the sintered samples (S1, S2, S3) were treated by heat treatment at 1500 ℃ to simulate the directional solidification process. Isothermal uniaxial compression tests of ceramic core samples were conducted on a Gleeble-1500D mechanical simulator. Weibull approach was used to describe the strength distribution of silica-based ceramic cores. As a result, the mean compressive strength of the sample (S0) is 40.43 MPa. The mean compressive strengths of the samples (S1, S2, S3) with heat treatment at 1500 ℃ are 54.34 MPa, 53.60 MPa and 53.81 MPa, respectively, which are significantly larger than that of S0. The mean elastic moduli of the samples (S1, S2, S3) with heat treatment at 1500 ℃ are 2726.39 MPa, 2855.91 MPa and 2797.14 MPa, respectively, which is significantly higher than that of S0. The refractory particle evolution of the ceramic core during the directional solidification process is analyzed, and the microstructural investigations show that the crack propagation of ceramic core sintered at 1000 ℃ is mainly through the sintering necks between particles. However, the crack propagation of ceramic core holding at 1500 ℃ is extended through the entire large particles. The re-sintering process of ceramic core holding at 1500 ℃ compensates the negative effect of cracks due to the volume contraction during β- to α-phase transformation and the rapid cooling process, and improves the ceramic core uniformity and mechanical properties.     

Advanced ceramics from a preceramic polymer and nano-fillers

A commercial silicone resin (“silicone”) filled with ceramic nanoparticles has been employed for the preparation of mullite and β-SiAlON ceramics. Dense, pure, crack free mullite were prepared by the heating in air of a mixture of silicone resin and alumina nanoparticles in the temperature range 1200–1550 °C. The high reactivity of Al₂O₃ towards silica, coupled with nanometric size, led to a large volume fraction of mullite crystals even at low firing temperatures (1250 °C). β-SiAlON ceramics were prepared by the heating of a mixture of silicone resin and fillers consisting of Al₂O₃ nanoparticles and Si₃N₄ and AlN microparticles, in the temperature range 1450–1550 °C in nitrogen atmosphere. The formation of SiAlON was found to be preceded by the formation of intermediate alumino-silicate phases like mullite and sillimanite, successively reduced (due to the carbon content of the ceramic residue of silicone resins) and nitrided. Although some oxide contamination was still present after the high temperature treatment, a high β-SiAlON yield (about 80%) was achieved. The use of nano-filled silicones provides a promising route for the fabrication of advanced ceramic components by exploiting polymer processing techniques, with the achievement of complex shapes.     

Preparation of epoxy-based insulator and optimization of its thermal property by Taguchi robust design method in double base propellant grain application

Taguchi method (orthogonal array, OA₉) was used to design an epoxy insulator by evaluating its glass transition temperature (T _g) for using in a double base (DB) propellant grain. In this design method, three epoxy resins based on diglycidylether bisphenol A (DGEBA), three polyamine curing agents and a DGEBA-based reactive diluent agent were used. The curing process of epoxy resins with polyamines was studied by Fourier transform infrared spectroscopy. The results showed that the curing process was completed at room temperature. The effects of four parameters including resin type, curing agent type, curing agent concentration and diluent quantity were investigated to design a resin formulation with a highest T _g after curing. The obtained results were quantitatively evaluated by the analysis of variance (ANOVA). The results of ANOVA showed that the highest T _g of 86.0 ± 9.0 °C was obtained for the optimum formulation of MANA POX-95 as epoxy resin, H-30 as curing agent and 52 phr H-30. The T _g measured by the experiment was 78.0 ± 0.9 °C. In addition, the single lap shear strength (adhesion strength) of the optimized insulator was measured at 13.66 ± 1.02 MPa. Pull-off test performed on the surface of DB propellant resulted a 1.935 ± 0.003 MPa adhesion strength.     

High-performance Al2O3 ceramics prepared by DCC-HVCI via microwave heating

A novel and rapid fabrication method for Al₂O₃ ceramics by the DCC-HVCI method via microwave heating was proposed. Effects of microwave heating temperature on coagulation time, micromorphology, as well as performance of the green body and ceramic sample were studied. As the microwave heating temperature rises, the coagulation time gradually reduced and compressive strength of green sample decreased while relative density and flexural strength of ceramics rose at the beginning and then dropped. The 50 vol.% Al₂O₃ suspension was coagulated and demolded after treating at 60°C for 800 s by microwave heating. The compressive strength of green samples reached 1.12 ± 0.13 MPa. The relative density of Al₂O₃ ceramic samples reached 99.39%. And the flexural strength of Al₂O₃ ceramics reached 334.55 ± 26.41 MPa. The Weibull modulus of Al₂O₃ ceramics reached 19. In contrast with the ceramic samples heated through water bath, the ceramic samples treated through microwave possessed uniform microstructures. Microwave heating could reduce the coagulation time by 77%. Meanwhile, it could significantly raise the compressive strength of green bodies by 65%. Additionally, it could increase the flexural strength of ceramics by 30%.     

Influence of post-etch cleaning and silane heat treatment on resin bond strength to silica-based leucite: an in vitro study

Adhesive cementation of bonded all-ceramic restorations is critical for their long-term clinical performance. The objective of this study was to evaluate the role of post-etch cleaning (PEC) and silane heat treatment on the micro-tensile bond strength of silica-based leucite (SBLE) ceramic when bonded to composite resin. Twenty-four blocks of SBLE ceramic (HeraCeram Press®, Heraeus Kulzer GmbH Grüner Weg 11 63450 Hanau) were fabricated and bonding surfaces were etched using 9.5% hydrofluoric acid. Six experimental groups were made from the various surface treatment combinations including: PEC (37.5% phosphoric acid for 1 min, rinsed with water for 20 s and ultrasonic bath immersion), silane application and silane heat treatment (100 °C for 5 min). An adhesive resin and a light-cured restorative composite were used to bond the ceramic and composite resin blocks under standard conditions. Three hundred and sixty specimen sticks (8 × 1 mm²) were subjected to micro-tensile testing. The means of the micro-tensile bond strength (μ-TBS) were analysed with ANOVA and Tukey–Kramer multiple comparison test. The specimens tested were assessed for mode of failure using scanning electron microscopy. The highest μ-TBS value (38.25 ± 3.40 MPa) of the specimen was achieved by PEC and heated silane. PEC and silane application showed statistically significant improvements in the μ-TBS (p < 0.01). The mean maximum difference was due to PEC (18.91 ± 3.70 MPa). In the surface treatment of SBLE ceramics, PEC had the most significant factor which affected the μ-TBS of resin composite.     

Microstructure evolution and mechanical properties of ceramic shell moulds for investment casting of turbine blades by selective laser sintering

Ceramic shell moulds fabricated by traditional shell-making technology have relatively low strength, and often crack during the casting process due to the low strength. In addition, the traditional shell-making process requires long period and high cost. In this work, qualified mullite ceramic shell moulds with enhanced strength were fabricated by selective laser sintering (SLS) combined with high-temperature sintering process. The effects of SLS process parameters on dimensions were investigated, and process optimization was proposed by orthogonal experiments. The effect of sintering temperature on strength at room temperature and 900?°C were studied. X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM) analysis suggested that mullitization behavior was influenced by sintering temperature. Furthermore, the content of mullite phase, mullite grain sizes, and mean length-diameter ratio of the mullite grains increased with the sintering temperature. Mechanical testing results showed that the samples sintered at 1610?°C had an excellent compressive strength of 99.01?MPa at room temperature and over 172.02?MPa at 900?°C. These values far exceed those of ceramic shell moulds fabricated by the traditional shell-making process (40.43?MPa).     

Characterization of a rigid silicone resin

Silicone resins have been used as binders for ceramic frit coatings and can withstand temperatures of 650°C to 1260°C. Conceptually, silicone resins can potentially be used as matrices for high temperature fiber‐reinforced composites. The mechanical and thermal properties of a commercially available silicone resin, Dow Corning® 6‐2230, were characterized. Neat 6‐2230 resin was found to have inferior room temperature mechanical properties such as flexural, tensile and fracture properties when compared to epoxy. The room temperature flexural properties and short beam shear strength of the silicone/glass composites were also found to be lower than those of epoxy/glass composite with similar glass content. However, the silicone resin had better elevated temperature properties. At an elevated temperature of 316°C, the retentions of flexural modulus and strength were 80% and 40% respectively of room temperature values; these were superior to those of phenolic/glass. Unlike the carbon‐based resins, the drop in flexural properties of the silicon/glass laminates with temperature leveled off with increase in temperature beyond 250°C. The resin weight loss at 316°C in 100 cm³/min of flowing air was small compared to other carbon‐based resins such as PMR‐15 and LaRC TPI. Only Avimid‐N appeared comparable to Dow Corning® 6‐2230.     

Analysis of failure mechanisms of Oxide - Oxide ceramic matrix composites

The failure mechanisms of Oxide-Oxide ceramic matrix composites AS-N610 were studied at both room temperature and high temperature using tensile and fatigue tests with and without lateral and laminar notches. The unnotched coupons had an average tensile strength of 423 MPa with elastic modulus of 97 GPa at room temperature showing a perfect elastic behaviour whereas the laminar notched samples shown similar strength of 425 MPa with elastic modulus (98 GPa) revealing pseudo-ductile behaviour. A reduction in tensile strength of the oxide ceramic matrix composites was observed at high temperatures. Thermal shock experiments revealed that the retained strength of the samples quenched from 1100 °C deteriorated by ～10 % (395 ± 15 MPa). In all samples, fracture origin was observed on the mid-plane showing a higher degree of fiber pull-out, delamination and pseudo ductile behaviour. Finite element analysis confirmed higher stress concentration on the areas of failures.     

High-toughness mullite ceramics fabricated by hot-press sintering of pyrophyllite and AlOOH at low temperatures

High-toughness mullite ceramics were fabricated through hot-press sintering (HPS) of pyrophyllite and AlOOH, which were wet-milled and well mixed using a planetary ball mill. The impacts of sintering temperatures and contents of AlOOH on mullite phase formation, densification, microstructure and mechanical properties in ceramic materials were investigated through XRD, SEM and mechanical properties determination. The results indicated that high-toughness mullite ceramics could be successfully prepared by HPS at temperatures higher than 1200°C for 120 min. Increasing the sintering temperature from 1000 to 1300°C significantly enhanced the flexural strength and fracture toughness of samples. The highest flexural strength of 297.97±25.32 MPa and fracture toughness of 4.64±0.11 MPa⋅m^1/2 were obtained for samples sintered at 1300°C. Further increase of temperature to 1400°C resulted in slight decrease of flexural strength and fracture toughness. Compared with the mullite ceramics prepared only using pyrophyllite as raw material, incorporation of AlOOH into raw material significantly increased the mechanical properties of final mullite ceramics. And stoichiometric AlOOH and pyrophyllite as starting material gave the best performance in fracture toughness. The high-toughness of mullite ceramics were ascribed to the high mullite phase content, fine mullite whiskers and in situ formed, intertwined three-dimensional network structure obtained through HPS at a low temperature of 1300°C.     

Investigation of microstructure evolution and properties in silica-based ceramic cores with alumina as a mineralizer

In this work, silica-based ceramic cores with alumina as a mineralizer were prepared via an injection molding method, and the effects of alumina on the microstructural evolution and properties at 1450°C (simulating the process of equiaxed castings) and 1550°C (simulating the process of columnar/single crystal castings) were investigated. It was found that alumina promoted the cristobalite crystallization of fused silica refractory during sintering but inhibited the devitrification rate in the subsequent heating. The flexural strength of silica-based ceramic cores at an ambient temperature and 1450°C improved with an increasing alumina content, whereas the opposite trend appeared at 1550°C. The creep resistances of silica-based cores were improved significantly and then slightly deteriorated with an increasing alumina content from 5% to 20%, depending on the competition effects of alumina hindering the viscous flow of liquid silica (favorable), but suppressing the devitrification rate (unfavorable). The results of this work show that silica-based cores need to follow different compositional design principles for equiaxed and columnar/single-crystal turbine blade castings.     

Analysis of Effect of Pressure and Heat on Mechanical Characteristics of Butt Fusion Welding of Polyethylene Pipes

The butt fusion process is one of the most effective processes in welding polyethylene pipes. The heating stage is the most important step in this process. In this investigation, while the main objective was to reduce the final bead's size of the weld, 9 different experiments with different heat and pressure conditions and equal timing for each heating stage were defined. Numerical modeling of Finite Element Method (FEM) of the heating process was carried out in the computer software considering governing physical conditions in the weld to determine heat distribution as well as primary bead geometry. Subsequently, the model was compared with results from experimentations. Cross-cut of the formed primary beads at the end of the heating process were prepared and compared with results from the model. To review final quality of the weld and its mechanical characteristics, all samples were welded under equal pressure conditions. Cross-sections of beads formed at the final stage as well as some samples for tension test and impact test from all welded areas were prepared according to standard for determination of mechanical characteristics and then compared with each other. From mechanical strength perspective, the weld formed in 210°C and 0.18 MPa pressure demonstrated higher values. However, impact strength in the weld formed in 180°C was higher. By reducing pressure in a specified heating process, value of impact energy required to break the piece was reduced. Mechanical strength in heating condition 240°C was lower than all other cases. As for geometry of the formed bead; its size in 180°C and 0.03 MPa pressure in the first stage of the heating process was smaller than other cases.     

Thermal conductivities and mechanical properties of AlN ceramics fabricated by three dimensional printing

AlN ceramics were successfully fabricated through a joint process of digital light processing (DLP) 3D printing technology and heat treatment at 1780 °C∼1845 °C. DLP is an addictive manufacturing process, enabling the near net shape fabrication. The AlN grains in this work developed well and there were small amounts of grain-boundary phases at the three-grain junctions. The particle size of AlN became larger and the densification increased with increasing sintering temperature. The pores of AlN ceramics also decreased, which led to the increase of thermal conductivity and flexural strength. The optimal thermal conductivity and flexural strength of AlN ceramic reached 155 W/(m·K) and 265 ± 20 MPa when sintered at 1845 °C.     

Densification,microstructure and properties of ultra-high temperature HfB2 ceramics by the spark plasma sintering without any additives

Ultra-high temperature HfB₂ ceramic with nearly full densification is achieved by using gradient sintering process of SPS without any additives. The effect of the sintering temperature on the densification behavior, relative density, microstructure, mechanical and thermionic properties is systematically investigated. The results show that the fast densification of HfB₂ ceramic occurs at the heating stage, and the highest relative density of 96.75% is obtained at T =1950 °C, P = 60 MPa and t =10min. As the temperature is increased from 1800 to 1950 °C, the grain size of HfB₂ increases from 6.12 ±1.33 to 10.99 ± 2.25 μm, and refined microstructure gives the excellently mechanical properties. The highest hardness of 26.34 ±2.1GPa, fracture toughness of 7.12 ± 1.33 MPa m^1/2 and bending strength of 501 ±10MPa belong to the HfB₂ ceramic obtained at T =1950°C. Moreover, both the Vickers hardness and fracture toughness obey the normal indentation size effect. HfB₂ ceramic also exhibits the thermionic emission characterization with the highest current density of 6.12 A/cm² and the lowest work function of 2.92 eV.