Adsorption of anionic polyelectrolyte on an SiC surface and effects on dispersion stability

Aluminum nitrate (Al(NO₃)₃) and sodium polystyrene sulfonate (PSS) were used to improve the dispersion of fine silicon carbide (SiC) powders. Effects of modification parameters on the viscosity of modified SiC slurry were studied by orthogonal experiments. Modified SiC slurry with the solid loading of 50 vol% reached the lowest viscosity of 34 MPa s. The adsorption processes of PSS on the as-received and Al(NO₃)₃ premodified SiC surface were investigated. The results indicated that the adsorption between PSS and premodified SiC surfaces was a high affinity type and was mainly controlled by active sites on an SiC surface. The Langmuir model and the pseudo-second-order model could better fit the adsorption isotherm and kinetics data, respectively. The contact angle decreased from 32.8 to 15.2° and the wettability was improved by modification. The isoelectric point of modified SiC powder shifted to the acidic region and the maximum zeta potential was obtained at pH 11. Sedimentation results also showed that a stable dispersed suspension of modified SiC was achieved at pH 11. Density–pressure curves demonstrated that the flowability and formability of SiC powder were improved by modification. The dispersion effect of PSS on SiC and Al₂O₃ composite powder was verified by viscosity and sedimentation results.     

Highly concentrated aqueous SiC slurry containing fine SiC powder: A new approach for ultra-dense green body

SiC slurry with ultra-high concentration up to 70 vol% was prepared using oxidized fine and coarse SiC powder mixture, and dense SiC green body with a relative density of 76% was fabricated by drying the slurry at ambient condition. Three approaches were performed to prepare highly concentrated SiC slurry; preparation of SiC powder having good dispersion behavior, optimization of the oxidation condition, and optimization of bi-modal particle size distribution. An aqueous slurry with the solid loading up to 62 vol% could be prepared using fine (150 nm) SiC powder prepared by the mechanical alloying of Si and carbon. The surface property of the fine and coarse (10 μm) SiC powders was optimized using an oxidation treatment. The maximum solid loading of the fine SiC slurry prepared using oxidized powder was 66 vol%. By optimizing the mixing ratio of the oxidized fine and coarse SiC powder to 75:25, the solid loading of the SiC slurry could increase up to 70 vol%. The relative densities of the green bodies after drying 66, 68, and 70 vol% slurries were 69, 75.7, and 76.1%, respectively, which values were higher than those (58%) prepared by cold isostatic pressing under 200 MPa.     

Preparation of photosensitive SiO2/SiC ceramic slurry with high solid content for stereolithography

Stereolithography is a popular three-dimensional (3D) printing technology, which is widely used for manufacturing ceramic components owing to its high efficiency and precision. However, it is a big challenge to prepare SiC ceramic slurry with high solid content for stereolithography due to the strong light absorption and high refractive index of dark SiC powders. Here, we propose a novel strategy to develop photosensitive SiO₂/SiC ceramic slurry with high solid content of 50–65 vol% by adding spherical silica with low light absorbance and applying a stacking flow model to improve the solid content of the slurry. The as-prepared slurry exhibits excellent stereolithography properties with a dynamic viscosity lower than 20 Pa s and curing thickness more than 120 μm. Therefore, it can be successfully applied for stereolithography-based additive manufacturing of SiC green bodies with large size (100 mm), sub-millimeter accuracy (0.2 mm), and complex structure. The stacking flow model also shows immense potential for the stereolithography of other dark-color ceramics with high solid content.     

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.     

Application of SiO2-coated SiC powder in stereolithography and sintering densification of SiC ceramic composites

Stereolithography additive manufacturing of SiC ceramic composites has received much attention. However, the forming efficiency and mechanical properties of their products need to be improved. This study aimed to prepare SiC ceramic composites with complex shapes and high flexural strength using a combination of digital light processing (DLP) and reactive solution infiltration process (RMI). A low-absorbance SiO₂ cladding layer was formed on the surface of SiC powder through a non-homogeneous precipitation process. With the densification of the cladding layer at high temperatures, SiO₂-coated SiC composite powder was used to formulate a photosensitive ceramic slurry with a solid content of 44 vol%. The resulting slurry exhibited a considerable improvement in curing thickness and rate and was used to mold ceramic green body with a single-layer slicing thickness of 100 μm using DLP. The ceramic blanks were then sintered and densified using a carbon thermal reduction combined with liquid silica infiltration (LSI) process, resulting in SiC ceramic composites with a density of 2.87 g/cm³ and an average flexural strength of 267.52 ± 2.5 MPa. Therefore, the proposed approach can reduce the manufacturing cycle and cost of SiC ceramic composites.     

陶瓷浆料用木质素系分散剂的性能及配伍研究

考察了改性木质素磺酸钠GCL3S系列产品对墙地砖陶瓷浆料应用性能的影响,结果表明,GCL3S具有较好的分散稳定性能。当低相对分子质量(以下简称分子量)的GCL3S-1掺量(分散剂占陶瓷粉料的质量分数,下同)为0.3%时,固含量(固体占陶瓷浆体的质量分数,下同)为71.26%的陶瓷浆料流出时间仅为41.79 s,厚化度为1.37;随GCL3S分子量增加,陶瓷浆料性能先提高后降低,重均分子量Mw=27 700的GCL3S-2对浆料的流动性及分散稳定性能最好。GCL3S产品与水玻璃、六偏磷酸钠、焦磷酸钠、三聚磷酸钠复配能进一步提高其应用性能,其中与六偏磷酸钠按质量比1∶1复配,总掺量为0.2%时,陶瓷浆料流出时间仅38.81 s,分散性能明显优于目前常用的无机盐分散剂。     

Polymer-metal slurry reactive melt infiltration: A flexible and controllable ceramic modification strategy for irregular C/C components

Herein, we investigate the applicability of the polycarbosilane (PCS)–metal slurry reactive melt infiltration (RMI) process to various metals. The slurry exhibiting the best ceramized ability was used to examine the relationship between the ceramic thickness and reactive time, ceramic thickness and reactive temperature, and infiltration depth and slurry-coating thickness. The results show that the thickness of the ceramic layer increases with reactive time and temperature and the infiltration depth increases with the coating thickness. PCS–Si₉₀Zr₁₀ slurry RMI was selected to modify cylindrical nozzle C/C preforms, and dense C/C–SiC–ZrC composites with a density of ~2.05 g cm⁻³ were obtained. Owing to the good control of the PCS–Si₉₀Zr₁₀ slurry RMI on the interface, matrix, and carbon fiber of the as-received cylindrical composites, the bending strength of the C/C–SiC–ZrC composites was as high as 306.4 MPa, which is considerably higher than that of a C/C preforms (70.4 MPa). Considering the ablation resistance, the mass and linear ablation rates of the C/C–SiC–ZrC composite (~0.29 mg s⁻¹ and ~2.48 × 10⁻³ mm s⁻¹, respectively) were similar to those of the composites prepared using traditional RMI (~0.23 mg s⁻¹ and ~2.29 × 10⁻³ mm s⁻¹). The proposed polymer–metal RMI is more suitable for the modification of C/C preforms with thin-wall structures owing to its advantages including precise control of infiltration dose and flexible operation of slurry coating. Furthermore, it is suitable for the local modification of C/C components.     

Dispersibility of pretreated polyacrylic acid-modified SiC powder

A slurry with high dispersibility is crucial for slip casting technology. The weakly acidic SiC powder with high dispersibility was prepared with polyacrylic acid pretreated by the sodium hydroxide (adjusted pH = 5). The pretreated polyacrylic acid can be effectively adsorbed on the surface of SiC powder, and its utilization efficiency (37%) was better than the unpretreated one (21%). The modified SiC powder with pH = 6 was obtained by polyacrylic acid modification, and the maximum solid content was 61.2 Vol%. The optimum of the pretreated polyacrylic acid addition amount was 1 wt% based on Zeta potential, solid content, and viscosity analysis data. Compared with the unmodified SiC, the Zeta potential absolute value of the modified (−63 mV) was higher due to a large amount of anionic modifier adsorbed on particle surfaces. The modified SiC slurry was more stable because the modification increases the electrostatic repulsion among the SiC molecules.     

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.     

Fabrication of 2D C/ZrC–SiC composite and its structural evolution under high-temperature treatment up to 1800 °C

Two-dimensional C/ZrC–SiC composites were fabricated by chemical vapor infiltration (CVI) process combined with a modified polymer infiltration and pyrolysis (PIP) method. Two kinds of ZrC slurries (ZrC aqueous slurry and ZrC/polycarbosilane slurry) were employed to densify composites before the PIP process. The as-produced C/ZrC–SiC composites exhibited better mechanical properties than the C/SiC composites densified only by CVI and PIP process. Structural evolution for C/ZrC–SiC composites treated in the range 1200–1800 °C mainly consisted of the change of SiC whiskers and the decomposition of polymer derived ceramic.     

Additive manufacturing of SiC-Sialon refractory with excellent properties by direct ink writing

Additive manufacturing of SiC-Sialon refractory with complex geometries was achieved using direct ink writing processes, followed by pressureless sintering under nitrogen. The effects of particle size of SiC powders, solid content of slurries and additives on the rheology, thixotropy and viscoelasticity of ceramic slurries were investigated. The optimal slurry with a high solid content was composed of 81 wt% SiC (3.5 µm+0.65 µm), Al₂O₃ and SiO₂ powders, 0.2 wt% dispersant, and 2.8 wt% binder. Furthermore, the accuracy of the structure of specimens was improved via adjustment of the printing parameters, including nozzle size, extrusion pressure, and layer height. The density and flexural strength of the printed SiC-Sialon refractory sintered at 1600 °C were 2.43 g/cm³ and 85 MPa, respectively. In addition, the printed SiC-Sialon crucible demonstrated excellent corrosion resistance to iron slag. Compared to the printed crucible bottom, the crucible side wall was minimally affected by molten slag.     

pH值对包覆改性SiC料浆分散特性和流变性的影响

通过zeta电位、沉降实验、流变特性、粘度等测试表征pH值对包覆改性SiC料浆分散特性和流变性的影响。研究表明:以偶联剂作为基础层,有机聚电解质作为分散功能层的有机包覆改性SiC粉体主要通过静电空间位阻效应实现稳定分散,调节pH值可以控制接枝聚合物水解产物的解离方式,从而改变了颗粒表面的电荷种类和电荷密度,包覆改性粉体的流动特性也发生变化。调整料浆pH值约11可制备出固相体积分数达56％、表观粘度为568 MPa·s的稳定料浆。     

Architectural engineering inspired method of preparing Cf/ZrC–SiC with graceful mechanical responses

Inspired by grouting technique in architectural engineering, an innovative method of slurry injection and vacuum impregnation was put forward to introduce nanosized ZrC–SiC ceramics into PyC modified 3-D needle-punched carbon fiber preform homogeneously and continuously, followed by spark plasma sintering to prepare C_f/ZrC–SiC with graceful mechanical responses. The composite possessed improved fracture toughness and work of fracture at 5.37 ± 0.25 MPa∙m^1/2 and 951 ± 12 J/m², 50% and nearly one order of magnitude higher than those of ZrC–SiC composite, respectively, with rivaling flexural strength at 177 ± 8 MPa synchronously. A graceful fracture mode was embodied in an obviously extended yield plateau with increased failure displacement by 300%. This enhancement was attributed to the uniform and continuous combination of ZrC–SiC with carbon fiber preform as well as protection and interface tailoring from PyC coating. The study offered an easy and effective method of preparing 3-D fiber reinforced ceramic matrix composites.     

Highly resistive SiC ceramics sintered with Al2O3-AlN-Y2O3 additions

A polycrystalline SiC ceramic prepared by pressureless sintering of α-SiC powders with 3 vol% Al₂O₃-AlN-Y₂O₃ additives in an argon atmosphere exhibited a high electrical resistivity of ~10¹³ Ω cm at room temperature. X-ray diffraction revealed that the SiC ceramics consisted mainly of 6H- and 4H-SiC polytypes. Scanning electron microscopy and high resolution transmission electron microscopy investigations showed that the SiC specimen contained micron-sized grains surrounded by an amorphous Al-Y-Si-O-C-N film with a thickness of ~4.85 nm. The thick boundary film between the grains contributed to the high resistivity of the SiC ceramic.     

Preparation of uniformly dispersed YAG ultrafine powders by co-precipitation method with SDS treatment

Uniformly dispersed yttrium aluminum garnet (Y₃Al₅O₁₂, YAG) ultrafine powders were synthesized by co-precipitating a mixed solution of aluminum and yttrium nitrates with ammonium hydrogen carbonate in the presence of sodium dodecyl sulfate (SDS) as dispersing agent. The primary purpose of introducing SDS was to protect YAG particles from agglomeration. The evolution of phase composition and micro-structure of the as-synthesized YAG powders were characterized by thermogravimetry/differential scanning calorimetry, X-ray diffraction, infrared spectra and scanning electron microscopy. The results showed that phase-pure YAG powders could be achieved by calcination of the precursor at 900 °C for 2 h. Uniformly dispersed YAG powders with a particle size of approximately 90-100 nm were obtained with optimum molar ratio of Al³⁺ to SDS at 2. And excessive SDS restrained good dispersion of the YAG powders. The dispersion mechanism of SDS in the preparation process was discussed.     

Fabrication of SiC reticulated porous ceramics with multi-layered struts for porous media combustion

Silicon carbide reticulated porous ceramics (SiC RPCs) with multi-layered struts were fabricated at 1450 °C by polymer sponge replica technique, followed by vacuum infiltration. The effect of additives (polycarboxylate, ammonium lignosulfonate and sodium carboxymethyl-cellulose) on the rheological behavior of silicon carbide slurry was firstly investigated, and then the slurry was coated on polyurethane open-cell sponge template. Furthermore, alumina slurry was adopted to fill up the hollow struts in vacuum infiltration process after the coated sponge was pre-treated at 850 °C. The results showed that the coating thickness on the struts and the microstructure in SiC RPCs were closely associated with the solid content of alumina slurry during vacuum infiltration. The typical multi-layered strut of SiC RPCs could be achieved after the infiltration of an alumina slurry containing 77 wt% solid content. The compressive strength and thermal shock resistance of the infiltrated specimens were significantly improved in comparison with those of non-infiltrated ones. The improvement was attributed to the in-situ formation of reaction-bonded multilayer struts in SiC RPCs, which were characterized by the exterior coating of aluminosilicate-corundum, middle part of mullite bonded SiC and interior zone of corundum.     

Synthesis,Characterization, and Microstructure of Hafnium Boride‐Based Composite Ceramics Via Preceramic Method

The ceramic precursor for HfB₂/HfC/SiC/C was prepared via solution‐based processing of polyhafnoxanesal, linear phenolic resin, boric acid and poly[(methylsilylene)acetylene)]. The obtained precursor could be cured at 250°C and subsequently heat treated at relative lower temperature (1500°C) to form HfB₂/HfC/SiC/C ceramic powders. The ceramic powders were characterized by element analysis, thermal gravimetric analysis, X‐ray diffraction, Raman spectroscopy, and Scanning electron microscopy. The results indicated that the ceramic powders with particle size of 200~500 nm were consisted of pure phase HfB₂, HfC, and SiC along with free carbon as fourth phase with low crystallinity.     

Dispersion and properties of zirconia suspensions for stereolithography

Stereolithography is an attractive technique for the fabrication of complex-shaped ceramic components with high dimensional accuracy. One of the challenges in this technology is the development of high solid loading, low viscosity photosensitive ceramic suspension. In this study, the dispersion of zirconia in photocurable resin and the slurry properties were intensively investigated. Rheological measurements showed that DISPERBYK-103 proved to be an effective dispersant. 42 vol% ZrO₂ suspension was successfully prepared using 3.5 wt% DISPERBYK-103 as the dispersant, with a suitable viscosity (4.88 Pa·s) below the maximum allowable viscosity value (5 Pa·s) for stereolithography applications. The adsorption behavior of DISPERBYK-103 on the surface of zirconia powders was characterized by TG and FT-IR, confirming the dispersion effect of dispersant. Contact angle measurements were also conducted to show that the adsorption of DISPERBYK-103 could help to improve the wettability between powder and photocurable resin. Results showed that DISPERBYK-103 was effective for the preparation of suitable slurries for the development of ZrO₂ ceramics through stereolithography.     

Effect of SiC powder on the properties of SiC slurry for stereolithography

Silicon carbide (SiC) is a kind of structural ceramics with excellent properties and it is widely used in industrial fields. Stereolithography (SL) is a potential additive manufacturing technique to fabricate fine complex SiC components, the resin-based SiC slurry with superior rheological and photo-polymerization properties is important for SL. In this paper, we investigated the influence of SiC powder on the properties of the SiC slurries for SL. The physical characteristics of SiC powder such as particle size, size distribution and appearance were tested and observed, and their influence on the dispersion, sedimentation and photo-polymerization property of the SiC slurry were investigated and discussed in detail based on their correlative theory, we finally prepared SiC slurry with superior rheological and photo-polymerization properties, and fabricated the fine complex SiC green body with low defects, high accuracy and high bending strength successfully. The SiC slurry with the solid content of 40 vol% was fabricated by the SiC powder with the median diameter D₅₀ ≈ 10.0 μm and a narrow particle size distribution, it is Bingham fluid with good fluidity and the viscosity of it is 464.40 mPa s under the shear rate of 51.08 s^?1, the cured SiC parts with Z – axis dimension change of 0.75% was finally fabricated, the three points bending strength of it is 50.18 MPa. Our research work provides some fundamental understanding of the SL technique for fabricating fine complex SiC components, explored a suitable way to fabricate high quality SiC green parts through SL, and offers some valuable references for preparing SiC slurry with superior rheological and photo-polymerization properties.     

Fabrication of modified ultra high-temperature ceramic hybrid powders using in situ grown SiC nanowires

Ultra-high temperature ceramic (UHTC) hybrid powders modified using in situ grown SiC nanowires (SiCNWs) were successfully prepared via a simple catalytic method. The self-produce carbon and silicon source promoted the growth of SiCNWs during the pyrolysis process of ZrB₂ polymer precursors coated ZrB₂-SiC powders. The results showed that the growth of SiCNWs could be explained by a tip-growth model and vapor–liquid–solid (VLS) growth mechanism. The SiCNWs with diameter of 200 nm were single crystalline, and the content could be controlled by changing the catalyst content.