Properties Of Green Bodies Research Articles

Influence of particle size and aggregates on translucent alumina ceramics fabricated by gelcasting

Three types of alumina powders and a polymer electrolyte Isobam system were used to fabricate translucent alumina ceramics via gelcasting, and each powder had the highest attainable solid loading. The effects of alumina particle size on slurry dispersion, microstructures and properties of green bodies and ceramics were investigated. All of the high-solid loading slurries contained strong aggregates, which could bridge with each other to form weak agglomerates. The smaller the initial particle size was, the more the contained particle number per aggregate. In addition, the smaller the aggregate size was, the lower the sintering activation energy of the ceramic and, finally, the higher the relative density. The initial particle size of the powder may not be the critical factor determining ceramic sintering, but the aggregate size and effective volume fraction of the aggregates may be the critical factors. Finally, the in-line transmittance of the ceramic with a higher density reached 22% at a wavelength of 650 nm and a thickness of 0.8 mm.

Tailoring calcination products for enhanced densification of Li7La3Zr2O12 ceramics

The densification of Ga-doped Li7La3Zr2O12 (LLZO) ceramics was optimized by controlling the phase chemistry and morphology of green powders after calcination. A solution-based approach was used to synthesize the green powders which were calcined at temperatures between 600 °C and 950 °C and free-sintered into dense pellets. The ionic conductivity and relative density were optimized at a calcination temperature of 700 °C to be 1.28×10−3 S/cm and 96.2%, respectively. At this condition, the green powder consisted primarily of La2Zr2O7 pyrochlore nanoparticles (80–100 nm) and LLZO particles (0.5–1 µm), which promoted reaction-driven densification and enabled a favorable bimodal size distribution for improved packing density. Further increasing the calcination temperature was correlated with a reduction in density due to the detrimental effects of particle coarsening on sintering activity. These findings show that controlling the calcination conditions is an effective method for tailoring green body properties for improved densification of LLZO.

Effect of Polymeric Binders on Green body Properties of WC-Co Cemented Carbides

Effect of Polymeric Binders on Green body Properties of WC-Co Cemented Carbides

Ceramic Stereolithography of Bioactive Glasses: Influence of Resin Composition on Curing Behavior and Green Body Properties.

Herein we report on the preparation of a bioactive glass (BAG)-based photocurable resin for the additive manufacturing of BAG scaffolds with high filler loadings. The preparation of glass/ceramics resins for stereolithography with high filler loading is always a challenge, especially for fillers with a high refractive index variance. Various photocurable resin compositions with and without bioactive glass fillers have been investigated to see the influence of bioactive glass on physical properties of the resin and resulting green body. The effect of concentration of monomers, reactive diluent, light absorber (Sudan orange G dye), photoinitiator (PI), non-reactive diluent, and fillers (BAG) on rheology and photocuring behavior of the resin and tomography of the resulting 3D structures have been investigated. The BAG contents affect the rheology of resin and influence the rate of the polymerization reaction. The resin compositions with 55–60% BAG, 10% PEG-200 (diluent), 1% of PI and 0.015% of the dye were found to be suitable compositions for the stereolithographic fabrication. A higher percentage of PI caused over-curing, while a higher amount of dye decreased the cure depth of the resin. The micro-computed tomography (µ-CT) and scanning electron microscopic (SEM) images of the resulting green bodies display a relatively dense glass scaffold without any visible cracks and good interlayer connection and surface finishing. These properties play an important role in the mechanical behavior of 3D scaffolds. This study will be helpful to prepare high density glass/ceramic slurries and optimize their printing properties.

In situ coagulation of yttria‐stabilized zirconia ceramic with enhancement of green body via polyvinyl pyrrolidone crosslink

ABSTRACTIn situ coagulation for yttria‐stabilized zirconia (YSZ) suspension via polyvinyl pyrrolidone (PVP) crosslink is reported. PVP is used to prepare sterically stabilized YSZ suspension. Influence of PVP on the dispersion of YSZ suspension was investigated. It indicates that well disperse YSZ suspension with 0.3 wt % PVP can be prepared. Dimethyl sulfate (DMS) was added at 40 °C to coagulate the suspension after degassing. Influence of DMS content and coagulation temperature on coagulation process and properties of green bodies were investigated. It indicates that sufficiently high viscosity to coagulate the suspension is achieved with the addition of 1 vol % DMS at 60~80 °C. The coagulation mechanism is proposed that the YSZ suspension is destabilized by the self‐crosslink of PVP. Coagulated samples with the highest wet compressive strength of 6.34 MPa could be demolded without deformation by treating 50 vol % YSZ suspension at 60 °C. Dense YSZ ceramics with relative density above 99.1% and flexural strength of 920 ± 90 MPa had been prepared by this method sintered at 1450 °C for 3 h. © 2020 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020, 137, 48889.

Cost effective preparation of Si3N4 ceramics with improved thermal conductivity and mechanical properties

High-purity silicon powder is used as the starting material for cost-effective preparation of silicon nitride ceramics with both high thermal conductivity and excellent mechanical properties using RE2O3 (RE=Y, La or Er) and MgO as sintering additives. Nitridation is a key procedure that would affect the properties of green bodies and the sintered samples. The β: (α+β) ratio can be increased as the samples nitrided at 1450ºC and a large amount of long rod-like β-Si3N4 grains were developed in the samples. It was found that the addition of Er2O3-MgO could help to improve the mechanical properties of the sintered Si3N4 ceramics, the thermal conductivity, flexural strength and fracture toughness of the sample were 90 W/(m∙K), 953±28.3 MPa and 10.64±0.61 MPa·m1/2, respectively. The RE3+ species with larger ionic radius tended to increase the oxygen of nitrided samples and decrease N/O ratio (triangle grain boundary) of sintered samples.

Transparent alumina ceramics: Effect of standard and plasma generated stabilizing approaches in colloidal processing

AbstractThe study is focused on an optimization of the slip‐casting process used for the fabrication of the transparent/translucent alumina ceramics; more precisely, on specifying the most appropriate way to stabilize the cast alumina suspensions. An innovative method of the particles’ stabilization by plasma treatment was compared with the classical electrostatic and the most frequently used electrosteric approach. Properties of green bodies (pore size distribution, density) and sintered samples (density, mean grain size, real in‐line transmittance) were measured in term to evaluate the impact of the individual stabilization mechanism on the final properties of the transparent/translucent ceramics. The results showed that all tested approaches enable the preparation of the transparent/translucent alumina ceramics by Hot Isostatic Pressing. Ceramics prepared from the plasma treated as well as the electrostatically stabilized powders exhibited narrower pore size distribution, higher density, and lower mean grain size in comparison to ceramics fabricated from only electrosterically stabilized powders. Despite these promising properties the plasma‐treated samples resulted in an unexpectedly low RIT of 36% caused by the presence of thin cracks. However, the electrostatically stabilized samples achieved the highest RIT value of 57%.

Gelcasting of Al2O3–W composites: Broadband dielectric spectroscopy and rheological studies of tungsten influence on polymerisation kinetics

Abstract Gelcasting is a method which allows for the production of high-quality ceramic-metal composites. In this work, the problem of local polymerisation in gelcasting of alumina-tungsten composite and metal influence on activation energy of glycerol monoacrylate was investigated. The broadband dielectric spectroscopy method was used for the first time to study the kinetics of gelation in ceramic processing. Polymerisation reaction rates constant of pure monomer, and monomer with ceramic and the metal filler, within the temperature range from 313 K to 333 K were determined. The obtained results were compared with rheological measurements. The calculated activation energy of polymerisation for monomer with 0.5 vol% of tungsten is 66 kJ/mol in comparison to a pure monomer which is 290 kJ/mol. This indicates the catalytic influence of metal on the polymerisation. Therefore, in the alumina suspension with tungsten polymerisation begins near the surface of the metal particles resulting in polymer structure inhomogeneity and lower mechanical properties of green bodies.

Design and formulation of polyurethane foam used for porous alumina ceramics

The present work studied a simple direct foaming method for preparation of porous alumina ceramics by expansion of a ceramic suspension based on polyurethane (PU) foam system. The effects of polyurethane formulas including catalyst composition, blowing agent content, NCO index and solid content on the samples properties were investigated. The results showed that the homogeneity, porosity and mechanical properties are various for different formulas. The dried green bodies showed diametrical compressive strength in the range of 0.39–1.25 MPa and were amenable to machining operations such as milling, drilling and lathing. Meanwhile, PU formulas play an important role in the microstructures and mechanical properties of green bodies and sintered ceramic foams. Pyrolytic removal of polyurethane skeleton followed by sintering at 1550 °C produced alumina bodies with open cell porosity 54–75% and diametrical compressive strength 1.39–28.47 MPa. Microstructure showed both large (200–300 μm) and small (50–100 μm) pores all with various sizes of windows. Based on the optimization of polyurethane formulation, the porous alumina foam with porosity of 64% and compressive strength of 25.26 MPa was prepared. This polyurethane foam system is easily available and low-cost, which could be widely applied in preparation of other porous ceramics, such as ZrO2, SiO2, etc.

Study of 0.9Al2O3\u20130.1TiO2 ceramics prepared by a novel DCC-HVCI method

In this paper, in-situ coagulation of 0.9Al2O3–0.1TiO2 suspension and microwave dielectric properties of 0.9Al2O3–0.1TiO2 ceramics prepared by a novel direct coagulation casting via high valence counter ions (DCC-HVCI) method were proposed. The 0.9Al2O3–0.1TiO2 suspension could be coagulated via controlled release of calcium ions from calcium iodate at an elevated temperature. The influence of tri-ammonium citrate (TAC) content, solid loading, and calcium iodate content on the rheological properties of the suspension was investigated. In addition, the influence of coagulation temperature on coagulation time and properties of green bodies was also studied. It was found that the stable 0.9Al2O3–0.1TiO2 suspension could be successfully prepared by adding 0.3 wt% TAC and adjusting pH value to 10–12 at room temperature. 0.9Al2O3–0.1TiO2 green bodies with uniform microstructures were coagulated by adding 8.0 g/L calcium iodate after treating at 70 °C for 1 h. 0.9Al2O3–0.1TiO2 ceramics, sintered at 1500 for 4 h and annealed at 1100°C for 5 h, showed °Cuniform microstructures with density of 3.62±0.02 g/cm3. The microwave dielectric properties of 0.9Al2O3–0.1TiO2 ceramics prepared by DCC-HVCI method were: εr = 11.26±0.06, Q×f = 11569±629 GHz, τf= 0.93±0.60 ppm/°C. The DCC-HVCI method is a novel and promising route without binder removal process to prepare complex-shaped microwave dielectric ceramics with uniform microstructures and good microwave dielectric properties.

In-situ coagulation of yttria-stabilized zirconia suspension via dispersant hydrolysis using sodium tripolyphosphate

A novel in-situ coagulation method without coagulation agent and adjusting pH value for yttria-stabilized zirconia (YSZ) suspension via dispersant hydrolysis is reported. Sodium tripolyphosphate (STPP) is used as dispersant to prepare electrostatic stabilized YSZ suspension. Influences of STPP contents on the dispersion and pH value of YSZ suspension were investigated. It indicated that there was a well-dispersed YSZ suspension with the addition of 0.3wt% STPP at pH=10. Influence of coagulation temperature on coagulation process and properties of green body was investigated. The sufficiently high viscosity suspension to coagulate was achieved at 60–80°C. The coagulation mechanism was different from traditional direct coagulation casting. The suspension was coagulated by directly shifting the isoelectric point to the original state without increasing the ionic strength and adjusting the pH value. It was proposed that the YSZ suspension could be destabilized via decrease of zeta potential by sodium tripolyphosphate hydrolyzing at elevated temperature. Coagulated samples with wet compressive strength of 3.60MPa could be demolded without deformation by treating 50vol% YSZ suspension with 0.3wt% STPP at 60°C for 30min. Dense YSZ ceramics with flexural strength of 887±110MPa and relative density of 98.9% had been prepared by this method sintered at 1450°C for 3h.

Temperature induced gelation of non–aqueous alumina suspension using oleic acid as dispersant

Abstract A novel temperature induced gelation method for alumina suspension using oleic acid as dispersant is reported. Non–aqueous suspension with high solid loading and low viscosity is prepared using normal octane as solvent. Influence of oleic acid on the dispersion of suspension was investigated. There was a well disperse alumina suspension with 1.3 wt% oleic acid. Influence of gelation temperature on the coagulation process and properties of green body was investigated. The sufficiently high viscosity to coagulate the suspension was achieved at −20 °C. The gelation temperature was controlled between the melting point of dispersant and solvent. The gelation mechanism is proposed that alumina suspension is destabilized by dispersant separating out from the solvent and removing from the alumina particles surface. The alumina green body with wet compressive strength of 1.07 MPa can be demolded without deformation by treating 53 vol% alumina suspension at −20 °C for 12 h. After being sintered at 1550 °C for 3 h, dense alumina ceramics with relative density of 98.62% and flexural strength of 371±25 MPa have been obtained by this method.

Rapid and uniform in-situ solidification of alumina suspension via a non-contamination DCC-HVCI method using MgO sintering additive as coagulating agent

Abstract A novel rapid, uniform and non-contamination in-situ solidification method for alumina suspension by DCC-HVCI method using MgO sintering additive as coagulating agent was reported. MgO was used to release Mg2+ in suspensions via reaction with acetic acid generated from glycerol diacetate (GDA) at elevated temperature as well as to improve density and suppress grain growth of alumina ceramics during sintering. Influence of adding 0.7 wt% MgO with 2.0 vol% GDA in alumina suspension on coagulation process and properties of green bodies and sintered samples were investigated. It was indicated that the controlled coagulation of the suspension could be achieved after treating at 70 °C for 10 min. Homogeneous composition distribution of Mg element in EDS result indicated the uniform solidification of suspensions. Compressive strength of wet-coagulated bodies is 2.09±0.25 MPa. Dense alumina ceramics with relative density of 99.2% and flexural strength of 354±16 MPa sintered at 1650 °C for 4 h present homogeneous microstructure. The result indicated that the novel DCC-HVCI method via a sintering additive reaction with no contamination, short coagulation time and uniform in-situ solidification is a promising colloidal forming method for preparing high-performance ceramic components with complex shape.

Reliability studies of gelcast fused silica between organic and inorganic binder systems

AbstractFused silica ceramics was prepared by using conventional organic binder, mathacrylamide‐N,N′‐methylenebisacrylamide (MAM‐MBAM) system by gelcasting process. Mechanical properties of green bodies were studied as a function of solid loading varying from 60 to 72 vol%. After evaluating the green body mechanical properties, the samples were densified at different sintering temperature from 1200 to 1450°C with definite intervals of 50°C and subjected to flexural strength analysis. Variation in flexural strength with sintering temperature was observed and correlated with the quantity of devitrification of fused silica during sintering. Quantification of devitrified cristobalite was carried out by using 20 wt% rutile (TiO2) as an internal standard by X‐ray diffraction. It was found that, as the cristobalite content increased, flexural strength decreased. Reliability studies were carried out for the samples having maximum flexural strength with and without crystalline content. Reliability studies have shown that for this organic binder system the sample sintered at 1300°C is crystalline free and most reliable product. The mechanical properties and reliability of this product processed with organic binder are compared with inorganic binder system. Results indicate that the sample fabricated using inorganic binder system is exhibiting high Weibull modulus and thus better reliability.

Chemo-Rheological Behavior of Aqueous Titanium Carbide Suspension and Evaluation of the Gelcasted Green Body Properties

Gel-casting is an advanced colloidal processing method for fabricating ceramic green parts. In this project acrylamide-based monomers were used as a gelcasting system. The effects of tetramethylammonium hydroxide and polyethylenimine dispersants on the premix solution containing titanium carbide powder have been studied via observation of the zeta potential and rheological behavior. The effect of various parameters on the gelation time and viscosity of solution and flexural strength and the shrinkage rate of titanium carbide green body were investigated. The results presented that the order of dispersion capacity of the tetramethylammonium hydroxide dispersant was better than the polyethylenimine dispersants. The results showed that the gelation time decreased and viscosity increased with increasing the monomer content, solid loading, initiator amount and temperature. The highest bending strength (39 MPa) was obtained for the samples containing 25 wt.% monomer content and 50% solid loading.

Preparation of silicon carbide ceramics using chemical treated powder by DCC via dispersant reaction and liquid phase sintering

Dense silicon carbide ceramics using chemical treated powder by DCC via dispersant reaction method and liquid phase sintering was reported. Ammonium peroxydisulfate ((NH4)2S2O8) and ammonium carbonate ((NH4)2CO3) were used as acid and base solutions to treat the silicon carbide powder, respectively. Influence of silicon carbide powder with chemical treatment on the preparation of silicon carbide suspension was studied. It was indicated that 50vol% and 52vol% silicon carbide suspensions with viscosities of 0.71Pas and 0.80Pas could be prepared using acid and base treated powders. Influence of silicon carbide powder with chemical treatment on the coagulation process and properties of green bodies and sintered ceramics were studied. It was indicated that silicon carbide green bodies with compressive strength of 1.13MPa could be prepared using base treated powder. Dense silicon carbide ceramics with relative density above 99.3% and flexural strength of 697±30MPa had been prepared by DCC via dispersant reaction and liquid phase sintering using Al2O3 and Y2O3 as additives at 1950°C for 2h.

2-carboxyethyl acrylate as a new monomer preventing negative effect of oxygen inhibition in gelcasting of alumina

The paper presents the application of 2-carboxyethyl acrylate as a new monomer in gelcasting of alumina. The research showed that the use of 2-carboxyethyl has a positive influence on the properties of green bodies, limiting the negative effect of oxygen inhibition. Oxygen inhibition which hampers polymerization reaction is a well known negative phenomenon in gelcasting but still not fully overcome for samples formed in air atmosphere. As a reference monomer 2-hydroxyethyl acrylate was used in the research. Rheological behavior of alumina suspensions containing both monomers has been studied, as well as the properties of green and sintered bodies obtained by gelcasting have been measured. The differences in the rheological properties and thus ceramic-monomer interactions in the slurries has been analyzed. The high values of densities and mechanical strength, accompanied with the pictures of microstructures of sintered ceramic parts have been presented, as a result of a successfully completed gelcasting process of alumina powder.

Starch Consolidation Casting of Cordierite Precursor Mixtures—Rheological Behavior and Green Body Properties

The rheology of suspensions and mechanical properties of green bodies with cordierite composition (raw materials 37 wt% kaolin, 41 wt% talc, 22 wt% alumina, resulting in 46.6 wt% SiO2, 38.1 wt% Al2O3, 13.6 wt% MgO) and two types of starch (corn or potato) are investigated. Rotational viscometry of suspensions with solids loading 50, 60, and 70 wt% without starch showed that all tend to be shear‐thinning with a small degree of thixotropy. Suspensions with a total solids loading of 60 wt% with 25 wt% replaced by starch exhibited higher viscosity and thixotropy, but the viscometric behavior is almost identical for the two starch types (apparent viscosities 130–50 mPa·s). Oscillatory rheometry shows that for suspensions with potato starch the onset temperature for gelatinization is 61°C–63°C, that is, lower than for corn starch (72°C–73°C). Maximum storage moduli and phase shift values after gelatinization are similar for both systems. The mechanical properties of green disks, measured via diametral compression tests, reveal clear differences between materials prepared with corn and potato starch, with the latter showing higher elastic modulus, higher strength, and higher deformation at fracture, obviously because of incompletely gelatinized starch granules in the green bodies prepared with corn starch.

Effect of solid loading on properties of Cr2O3 refractories by aqueous gelcasting

Dense chromic oxide refractories were prepared by aqueous gelcasting process. Effect of solid loading on rheological property of slurries, properties of green bodies and sintered bodies were investigated. AN-2000 was selected as the dispersant for obtaining slurries with high solid loading and low viscosity. The solid loading of suspension that can meet the requirement for casting was as high as 52 vol%. However, it was found that the highest relative density of the green body and the sintered body separately reached 66·17% and 85·38% when the solid loading came to 50 vol%, while the flexural strength of them were 13·60 MPa and 62·71 Mpa. Once the solid loading increased to 52 vol%, the relative density and mechanical properties of the green body decreased noticeably, which caused by the increase of the slurry viscosity. Besides, SEM images proved that green bodies and sintered bodies had the homogeneous microstructure when the solid loading was 48-50 vol%. As the solid loading was 52 vol%, hard agglomerations and pores formed in the green body, which had a significant influence on the properties of the sintered body.

Analysis of iron powder design for compaction process

This paper aims at finding a relationship among the iron powder design parameters, the material properties, and the final properties. The iron powder design parameters were the composition of graphite, particle size, and the composition of lubricant. The material properties in Shima–Oyane constitutive model are α, β, γ, a, b, and n. The final properties of green bodies are green density, density deviation, effective stress, hydrostatic pressure, effective strain, and volumetric strain. The correlations between the powder design parameters and the material properties were obtained by compaction experiments with regression method. The correlations between the material properties and the final properties were obtained by the compaction simulation with regression method. The regression model which shows the correlations between the powder design parameters and the final properties with the fixed process conditions and geometry were developed. This regression model gives the generic information of the powder design.