Green State Joining of SiC without Applied Pressure

External pressure (uniaxial or isostatic) is usually necessary to form a thin and defect-free joint in green state joining of SiC ceramics. A successful method of joining SiC in the green state using a liquid polymer precursor, allylhydridopolycarbosilane (AHPCS), without applied pressure, is described. The thermal decomposition behavior of the polymer was examined, and defect formation during joint evolution was investigated by interrupting the heat treatment at various stages. Cracks and pores were observed in the joints formed by pure AHPCS during the pyrolysis of the polymer precursor. Adding SiC powder to the joining paste eliminated defect formation. Optimum SiC loading in the paste was determined to be in the range of 25–35 vol%. Joints formed by AHPCS + (SiC + 5 wt% B) paste were essentially indistinguishable from the matrix and had an average strength of 323 MPa, comparable to that of the control sample.     

Green State Joining of Silicon Carbide Using Polycarbosilane

Green state joining of SiC was investigated using a paste consisting of polycarbosilane polymer and SiC powder. The joining process and densification were described. Initial experiments resulted in the formation of symmetrical black bands and cracks on both sides of the joint. However, with modifications in processing conditions, the cracks were eliminated and the resulting joints were indistinguishable from the matrix. The flexural strength of joined samples was measured to be 234 MPa, which was comparable to that of the control sample with similar density. As the applied pressure during joining was increased from 34 to 138 MPa, the strength of the joined samples increased from 180 to 250 MPa.     

Fabrication of membranes and microchannels in low-temperature co-fired ceramic (LTCC) substrate using novel water-based sacrificial carbon pastes

In this work, 3D structuration of LTCC (low-temperature co-fired ceramic) for microfluidics was studied, using two novel sacrificial carbon paste compositions. These pastes are based on graphite with a water-soluble vehicle consisting of polyvinylpyrrolidone binder (PVP) dissolved in propylene glycol (PG), which is not aggressive to green LTCC material. Both examined pastes differ slightly in binder content and added plasticizer, glycerol (G) or trimethylolpropane (TMP). The thermal properties of the sacrificial carbon pastes have been examined using combined thermo-gravimetric analysis (TGA), differential thermal analysis (DTA) and differential thermo-gravimetry (DTG). The sacrificial carbon pastes have been applied to the fabrication of membranes and microchannels in LTCC substrate. A comparison of the obtained features has been made using X-ray tomography and optical profile measurements. Moreover, changes in the composition of the fired LTCC material after co-firing have been studied using X-ray photoelectron spectroscopy (XPS) and surface wettability measurements.     

Joining oxide ceramic matrix composites by ionotropic gelation

The production of complex-shaped all-oxide ceramic matrix composites (Ox-CMC) is somewhat restricted by their current processing methods, as well as by the lack of applicable joining techniques. Thus, we present a new method for joining Ox-CMCs based on the gelation of slurries with the polysaccharide polymer alginate. For this investigation, Nextel 610/alumina-zirconia composites were produced using alginate as binder and aluminum acetate as gelling agent. The joining capabilities of this technique were investigated with microstructural analyses and single-lap compression shear tests. For that, a slurry-containing alginate was used to join two composite plates at different stages of the processing: gel state, dried green body and after sintering. Joining composites plates in their gel or green state was successful as the joints showed shear strength values similar to the interlaminar shear strength of the composites plates. The quality of the joints was attributed to the interactions between the alginate chains of the composite plates and the joint. We also show that even the joining of already sintered Ox-CMCs is feasible. However, densification cracks and lower shear strength are observed for such cases.     

Joining of zirconia ceramics in green state using a paste of zirconia slurry

A new technique for the green state joining of zirconia ceramics has been developed simply by using a paste of zirconia slurry. The interlayer of the joints has the same composition as the parent green bodies and, therefore, the mechanical properties of the joint are comparable to those of the bulk materials. Using this method, large and/or complex ceramic components could be produced cost effectively, because it minimizes the machining of the sintered body and eliminates the need for special equipment. This process can be applied to the joining of various other advanced ceramics.     

Physicochemical characteristics of acrylic-acid polymer-impregnated cement pastes

Various Portland cement pastes were made using water cement ratios of 0·20, 0·25, 0·35 or 0·40 and then cured for 1, 3, 7, 28, 90 or 180 days. These pastes were impregnated with acrylic acid monomer under vacuum and the monomer-impregnated samples were then treated at two different temperatures, 40 or 60°C, for the polymerization process, using benzoyl peroxide as initiator. Several physicochemical studies were carried out on each cement paste; these studies include compressive strength tests, bulk density, compressive strength versus gel/space ratio relationships, polymer load, X-ray diffraction analysis and differential thermal analysis. Results have indicated that compressive strength improvement in acrylic acid-polymer impregnated cement pastes is mainly dependent on initial water/cement ratio, curing time and gel/space ratio. The results of X-ray diffraction analysis and differential thermal analysis indicated that the intrusion of polymer into the cement paste matrix does not affect the phase composition of the Portland cement hydration products.     

Facile joining of SiC ceramics with screen-printed polycarbosilane without pressure

Joining of SiC ceramics was successfully achieved at a relatively low temperature of 1500 °C without any pressure using pure polycarbosilane (PCS) as the joining material, which was distributed homogenously on the surface of SiC monolith through a screen printing method. The XRD pattern shows that the pyrolysis product of PCS is single-phase SiC. The interlayer thickness of the SiC joint is approximately 2 μm. This ultra-thin interlayer with lower possibility of the existence of defects contributes to the average shear strength of 105.8 ± 10.4 MPa, higher than that of other works using other preceramic polymers to the best of our knowledge. Due to the simplicity, low cost and high joining strength, the screen printing method using PCS as the joining material has good practicality in SiC ceramics joining.     

Density Gradients and Sintered Dimensional Tolerance in Compacts Formed from Spray-Dried Alumina

This study proves that initial density gradients have lasting detrimental effects on final dimensional tolerances. X-ray computed tomography has been used to quantify changes in density following sintering; associated dimensional changes have been monitored using a laser micrometer. Nonuniformities present in the green state are still present at an overall relative density of ∼73%; in fact, these nonuniformities are exaggerated. Major losses of dimensional tolerance are triggered by the initial density gradients.     

Laser-supported joining of SiC-fiber/SiCN ceramic matrix composites fabricated by precursor infiltration

SiC-fiber/SiCN ceramic matrix composites were manufactured by means of polymer infiltration and pyrolysis. The fiber preform was made by slurry infiltration and winding using a computer-controlled winding module. Multiple infiltration steps using a Si–C–N precursor were included to increase the density. The influence of the sintering conditions on the microstructure of the CMC was demonstrated.Pipe sections made of the CMC materials were joined using a laser-supported heating technology with an Y–Al–Si–O glass–ceramic filler. The thermal response of the CMC components was controlled by the anisotropic thermal conductivity. Fast heating by laser beam was achieved for elements rotating in the direction of the fiber winding. SEM micrographs of the joints showed the good wettability of the CMC by the glass–ceramic filler. Nearly defect-free joints were obtained using a nitrogen process atmosphere. The laser-supported technology was shown to be promising for the joining of CMC components.     

注射成型物结构与性能的层析图像法研究

基于聚合物成型机理的三维层析数字图像化原理，对注射成型聚合物进行了X射线层析图像实验，在实验的基础上，详细分析了注射成型中聚合物层析结构形态特点，并从实验和理论两方面获得注射成型聚合物层析结构与其物理特性－－密度及其分布和取向之间的关系。     

Effects of the joining process on the microstructure and properties of liquid-phase-sintered SiC-SiC joints formed with Ti foil

The joining of liquid-phase sintered SiC (LPS-SiC) ceramics was conducted using spark plasma sintering (SPS), through solid state diffusion bonding, with Ti-metal foil as a joining interlayer. Samples were joined at 1400 °C, under applied pressures of either 10 or 30 MPa, and with different atmospheres (argon, Ar, vs. vacuum). It was demonstrated that the shear strength of the joints increased with an increase in the applied joining pressure. The joining atmosphere also affected on both the microstructure and shear strength of the SiC joints. The composition and microstructure of the interlayer were examined to understand the mechanism. As a result, a SiC-SiC joining with a good mechanical performance could be achieved under an Ar environment, which in turn could provide a cost-effective approach and greatly widen the applications of SiC ceramic components with complex shape.     

Processing of Cf/SiC composites by hot pressing using polymer binders followed by polymer impregnation and pyrolysis

Continuous carbon fiber (C_f) reinforced silicon carbide (SiC) matrix composite (C_f/SiC) was processed through hot pressing (HP) using polycarbosilane (PCS) in matrix and polysilazane in interphase regions as polymer binders. HP experiments were conducted at 4 MPa, 1200 °C and 1 h; followed by PCS polymer impregnation and pyrolysis (PIP) at 1200 °C under vacuum. The BN/SiC-Si₃N₄ interphase formed on the C_f cloth during BN dispersed polysilazane polymer coating and pyrolysis. The influence of PCS quantity during HP experiments on C_f/SiC composites was studied. Results suggest that sintering of SiC matrix in C_f/SiC composite improves by increasing PCS content during HP; however, high PCS content increases the liquidity of SiC-PCS mixture to flow out of the composite structure. The C_f/SiC composites with relative density ranging from 79 to 83% and flexural strength from 67 to 138 MPa was achieved.     

Effect of curing time on the physicomechanical characteristics of the hardened cement pastes containing limestone

The effect of curing time on the physico-mechanical properties of the hardened Portland cement pastes containing limestone was studied. Five cement-limestone blends were prepared using 0%, 5%, 10%, 15%, and 20% of limestone as a partial substituent of Portland cement. The cement pastes were prepared using the standard water of consistency of 0.255, 0.255, 0.258, 0.261, and 0.263, respectively. The fresh pastes, thus produced, were moulded into 2×2×2-cm cubes. The pastes were first cured within the moulds at 100% relative humidity for 24 h, then the specimens were demoulded and cured under tap water for 3, 7, 14, and 28 days. At each hydration age, the hardened pastes were tested for bulk density, compressive strength, differential scanning calorimetery (DSC), and X-ray diffraction analysis (XRD). The results obtained were related as much as possible to the mechanical properties of the hardened cement pastes. The inclusion of limestone results in a notable improvement of the mechanical properties of the cement pastes containing limestone.     

Pressure-less joining of alumina ceramics by the reaction-bonded aluminum oxide (RBAO) method

The present work demonstrates a pressure-less and reliable joining technique for alumina ceramics through a reaction-bonded aluminum oxide (RBAO) method. Effective joining relies on the RBAO mechanism, in which Al particles are converted to alumina through oxidation and bond with alumina particles from the parts to be joined upon sintering. Alumina ceramics in a green state were successfully joined with the use of an Al/Al₂O₃ powder mixture as an interlayer. The oxidation behavior of the Al particles was confirmed by thermogravimetry and X-ray diffraction analyses. Joining was performed in ambient air at 1650 °C for 2 h without applying any external pressure. Microstructural observations at the joining interfaces indicated a compact joining. The joining strengths were assessed by determining the biaxial strengths at room temperature, and the joined samples exhibited no fractures at the joining interfaces. Moreover, the joints had a strength of almost 100 % when compared with those of the parent alumina ceramics.     

Postcasting Contraction: Improving the Density of Gelcast Nanoparticle Green Bodies with Heated Liquid Desiccants

To achieve high‐density green bodies, a novel route without needing high solids loading suspensions, that is postcontraction process has been developed. In this process, the wet green body is immersed in heated liquid desiccants (polyethylene glycol [PEG] aqueous solution), which is prepared by gelcasting with thermoresponsive gel system. The density of green bodies is improved through releasing water quickly and shrinking rapidly. It is attributed to the cooperative action of the interior aggregation forces stemming from the shrinkage of network‐structured polymer and the exterior osmotic pressure from PEG aqueous solution. Alumina nanoparticle green bodies with different solids loadings were prepared by gelcasting with PNIPAM Poly(N‐isopropylacrylamide) gel system. The postcontraction process was almost completed in 30 min in liquid at 50°C, and meanwhile the bodies were almost dried. The relative densities of all green bodies and sintered parts are in accordance with each other, around 43% and 94%, respectively.     

Processing of Tape–Cast Laminates Prepared from Fine Alumina/Zirconia Powders

This paper addresses the effect of thermocompression pressure, shear deformation of green laminates, and postsinter HIPing on the microstructural homogeneity of cast tapes and laminates prepared from fine Al₂O₃, and Al₂O₃/ ZrO₂, powders. Green density increases with increasing thermo–compression pressure. Sintered densities, however, depend more on the macroscopic uniformity in the green tapes. When density gradients develop within the individual green tapes (because of improper drying), sintering is constrained in two dimensions and densities remain low. Postsinter HIPing does not significantly increase the sintered densities because of the retention of open porosity within the individual tape–cast layers. The use of a revised thermocompression process involving shear deformation results in higher sintered densities and complete densification after HIPing. Sintered densities increase with the degree of shear strain during green–state deformation processing. Thus, green-state deformation can improve homogeneity in laminates. A further variation of the shear deformation process has also been developed that allows the formation of complex shapes from tape–cast laminates in the green state, while retaining layer integrity.     

Estimation of ammonium perchlorate in HTPB based composite solid propellants using Kjeldahl method

Kjeldahl method has been applied to determine the percentage of ammonium perchlorate (AP) in hydroxy-terminated polybutadiene (HTPB) based composite solid propellants. It has been found that in pastes containing aluminium (Al) it is important to eliminate all the Al before starting the actual reaction (distillation). The results obtained are in the range of ±0.05% for pastes with and without Al whereas the range is ±0.02% for pure AP. End points are confirmed using pH meter.     

Joining of SiCf/SiC using polycarbosilane and polysilazane preceramic mixtures

Polycarbosilane (PCS)/polysilazane (PSZ) preceramic mixtures with weight ratios of 100/0, 75/25, 50/50, 25/75, and 0/100 were used as a filler for the joining of SiC_f/SiC to obtain high purity SiC at the joining region. SiC_f/SiC was fabricated by the electrophoretic infiltration of a SiC-based matrix phase into Tyranno SA3 SiC fabrics followed by hot-pressing at 1750?°C under 20?MPa for 2?h in an Ar atmosphere. Microstructural analysis confirmed a sound join without cracks after joining at 1750?°C for 2?h under a pressure of 10?MPa. SiC was the only phase remaining at the joint when PCS was used, while a small amount of Si₃N₄ along with the main SiC were observed in the join using PSZ. The flexural strengths of the butt-joint SiC_f/SiC were 120 and 137?MPa for the samples joined using a pure PCS and PSZ at 1750?°C, respectively, whereas those joined using the mixture fillers showed relatively lower strength.     

Microstructure characterization and compressive performance of 3D needle-punched C/C–SiC composites fabricated by gaseous silicon infiltration

3D needle-punched C/C-SiC composites were fabricated from carbon fiber reinforced carbon (C/C) preforms, with densities of 1.05?g/cm³ and 1.28?g/cm³, by the gaseous silicon infiltration (GSI) method at fabrication temperatures from 1500?°C to 1800?°C. The compressive strengths and elastic moduli in transverse direction are larger than those measured under longitudinal compression except that samples fabricated from 1.28?g/cm³ density exhibit lower elastic moduli in transverse direction than in longitudinal direction. The compressive strength and modulus increase with fabrication temperature at 1500?°C and 1600?°C, and then decrease with higher fabrication temperature. Samples fabricated from the lower density C/C preforms have greater compressive strength and modulus. X-ray tomography was applied before and after the mechanical tests to characterize the microstructure and damage patterns, and the results indicated that for C/C-SiC composites fabricated at 1700?°C from 1.28?g/cm³ density C/C preform the matrix has a volume fraction (vol%) of 36.9%, and the initial intra-bundle cracks (0.6?vol%) display a space crossing structure while the inter-bundle pores (6.0?vol%) are special irregularly distributed.     

Synthesis of centimeter-scale monolithic SiC nanofoams and pore size effect on mechanical properties

By pressure infiltrating pre-ceramic polymer polycarbosilane (PCS) into thermally and mechanically stable silica nanofoam, followed by PCS pyrolysis and silica template removal, synthesis of large-scale monolithic SiC nanofoams has been accomplished. Tailoring of the porosity and cell size of the SiC nanofoam has been realized by dissociating the porosity and pore size of the silica nanofoam. Because of the surface hardening and increased surface volume ratio of deformable nanopores, with the same porosity, the decrease of nanopore size has led to an increase in the quasi-static and dynamic indentation resistance for SiC nanofoams.