Gel-tape casting as a novel method for the production of flexible fine-grained alumina sheets

The paper reports on the development of a new aqueous gel-tape casting method for processing nanosized powders into thin fine-grained sheets with a high relative density after sintering. The method was based on casting a low-viscosity slurry into a tape, using the doctor-blade method and gelling the slurry after the casting. The gelled tape was removed from the tape carrier without any solvent evaporation and the drying of the gelled tape was performed later in a climate box under controlled temperature and humidity. The epoxy-based ceramic slurry could be prepared with a solid loading of 42 vol.%. Ceramic sheets with flat and smooth surfaces were prepared in a thickness range from 0.08 to 0.4 mm after sintering. The sintered sheets reached a relative density of 99.4%, with an average grain size of about 1.1 μm. The strength and flexibility of alumina sheets were investigated and discussed.     

Fabrication of porous titania sheet via tape casting: Microstructure and water permeability study

In this article, we report the effects of slurry formulation and sintering conditions on the microstructure and permeability of porous titania sheets prepared by tape casting. It was found that solid concentration and binder content in the titania slurry play a vital role in the porosity and microstructure of the sintered titania sheets. Solid concentration and binder content were optimized based on the green tape quality and open porosity of the sintered titania sheets. The optimum solid concentration with the lowest surface roughness was obtained at 0.61 g/cm³. The effects of temperature and sintering time on the open porosity and crystal structure of the final product were also investigated. Increasing the sintering temperature from 1000 to 1100 °C resulted in increasing the pore size from 170 to 264 nm and decreasing the open porosity. Finally, water permeability of the porous titania sheets was studied to evaluate the permeation flux and maximum operating pressure. The results revealed that the permeability of the porous titania sheet is increased not only by increasing the open porosity but also by increasing the pore size.     

分散剂对低温共烧陶瓷流延浆料流变性能的影响

本文探究了蓖麻油、BYK-22552、聚乙烯吡咯烷酮(PVP)、TEGO-700四种分散剂对CaO-B₂O₃-La₂O₃玻璃/氧化铝低温共烧陶瓷(LTCC)流延浆料分散性的影响,并进一步对该体系浆料流变性能、触变性能、固相体积分数以及沉降性能方面进行了研究,通过红外光谱分析研究了四种分散剂的分散机理并给出了解释。结果表明,当分散剂TEGO-700用量为粉体质量的2%时,流延浆料具有最小黏度(1 650 mPa·s)与最佳触变恢复性。在流延成型最佳黏度2 000 mPa·s下,浆料具有最大固相体积分数(37.2%)与优异的沉降性能。该浆料流延成型得到的柔性生瓷带表面平整且厚度均一,表面粗糙度为144 nm。烧结得到的基板材料表面无气孔、裂纹等明显缺陷,烧结致密化程度高,表面粗糙度为210 nm,40 GHz下测得介电常数与介电损耗分别为6.257和1.431×10^-3。     

Ceramic domes fabricated by a combination of tape casting and vacuum forming

Tape casting is a low cost fabrication process for flat ceramic sheet and this paper demonstrates how it can be combined with vacuum forming to make α-alumina domes of 250-300 μm sintered thickness. The suspension formulation makes use of systems of double plasticizers and double solvents in a poly(methyl methacrylate) binder to provide plastic ceramic films by tape casting from which preforms for vacuum forming were cut. In order to retain the shape of vacuum formed domes during debinding and sintering, an initial low temperature anneal is needed. The study indicates that the ratio of plasticizers to binder and the particle size are two dominant parameters in influencing the elongational flow. The whole process provides a novel method to make thin ceramic domes.     

Influence of Green Formulation and Pyrolyzable Particulates on the Porous Microstructure and Sintering Characteristics of Tape Cast Ceramics

Porous morphology and total porosity produced in sintered ceramic tapes was controlled by the amount and distribution of pyrolyzable graphite particles added to a colloidal suspension during a tape casting operation. A conceptual model of the green tape microstructure was used to explain the influence of graphite and tape formulation on sintering characteristics. The creation of a connected, open porous network in the sintered body was the result of graphite particle percolation within the green body. Additional voidage introduced by particle bridging was the source of excess porosity and also resulted in a bimodal pore size distribution. Sintering shrinkage was determined by the ceramic packing density, which was primarily determined by the tape formulation.     

流延法制备8YSZ薄膜

采用非水基流延法制备了8mol%氧化钇稳定氧化锆薄膜,研究了球磨时间、固含量、有机添加剂含量及除泡工艺对8YSZ浆料流变性能的影响,通过SEM表征烧结体表面形貌,用电化学阻抗仪对烧结体进行电导率测试。结果表明:分散剂用量1.25wt%,球磨时间15h,浆料的粘度最小,分散效果最好;增塑剂与粘结剂比例为0.7,粘结剂加入量6.5～8.5wt%,二次球磨后,真空除泡可获得适合流延的浆料;生坯1450℃烧结4h,烧结体晶界清晰、致密度较好;烧结体在300～800℃随温度的升高电导率逐渐增大,在800℃时离子电导率达0.046S/cm。     

Porous asymmetric microfiltration membranes shaped by combined alumina freeze and tape casting

An assembled asymmetric alumina microfiltration membrane with high performance was prepared by combining freeze and tape casting techniques followed by two sintering steps. Freeze casting was used for manufacturing of the porous support layer with a highly interconnected pore network. Tape casting was applied on the top layer to form a pre-membrane with smaller pore size and controlled thickness, which was set on the sintered support. Morphology influences were investigated for different solid loadings, additives content and the assembled layer membrane structures. No delamination among the layers was observed. The assembled ceramic membrane had an average pore size between 30 and 50 μm together with a top surface layer around 0.35 μm, which is suitable to the microfiltration separation process. Porosity in the range of 26–50 % and water flux of 11–32 m³ m^?2 h^?1 bar^?1 were reached for samples prepared with two sintering steps at 1600 and 1300 °C for 2 h.     

5YSZ陶瓷基体的成型及烧结收缩率调节

为了提高5YSZ陶瓷基体的致密度和调节其烧结收缩率,通过流延法成型,优化了分散剂、消泡剂、球磨时间、固含量和胶含量。优化的条件为:分散剂含量0.9%,消泡剂含量0.63%,球磨时间22h+22h,固含量64%,胶含量29%。在优化的条件下,浆料分散均匀,生瓷带无气泡,5YSZ陶瓷基体烧结致密,且与Al2O3印刷层共烧良好。     

UV Curable Systems for Tape Casting

The substitution of solvents by photopolymerizable binders in the tape casting process allows to achieve high ceramic loading and to eliminate the drying stage which is a critical step of the tape casting process. After the rapid UV polymerization of the resin, the high strength green tapes can be debinded and sintered. Ceramic suspensions containing alumina or zirconia powder, dispersant, UV curable binder and photoinitiator have been prepared. The use of a low viscosity organic vehicle allows to prepare low viscosity ceramic suspensions, containing about 50 vol% powder, which have a shear thinning behaviour. Because of the rapid attenuation of the incident light in UV curing systems containing ceramic particles it is important to estimate the thickness of the tape that can be treated. The effect of incident energy, of photoinitiator concentration and of powder volume fraction was studied. There is an optimal photoinitiator concentration which maximizes the cured depth and which depends on the volume fraction of solid. A theoretical model based on the Beer–Lambert’s law enables the prediction of cured depth for any volume fraction of solid. To prove the ability to manufacture ceramic sheets by tape casting, some suspensions were tape cast.     

The preparation of SiCP/Ag–Cu–Ti hybrid tapes and application in the joining of silicon carbide ceramics

Abstract

A novel method of tape casting to fabricate ceramic-particulate-reinforced composite filler alloy tapes with low organics (no more than 6?wt.%) was developed, with which SiC_P/Ag–Cu–Ti hybrid tapes were successfully prepared and used in joining of sintered silicon carbide ceramics. The stress rheometer, scanning electron microscopy and energy dispersive spectrometer were used to characterize the rheological properties of slurry and microstructure of green tapes and joints. The slurry for tape casting consists of dispersant, binder, solvent, a mixture of ceramics particulates and metal powders, and no plasticizer was added. Castor oil phosphate was proven the suitable dispersant for the slurry, and the content of dispersant, binder, solid loading was optimized as 3?wt.%, 2.6?wt.% and 26?vol.%, respectively. The fabricated hybrid tapes possess good ductility and uniform thickness. The SiC particulates were homogeneously distributed in the metal powders matrix in both sides of the green tapes, and the distribution was retained in the SiC/SiC joints.     

Production of Si3N4/Glass Composites for LTCC Substrate by Aqueous Tape Casting Process

In this work, Si₃N₄/glass sheets were prepared by aqueous tape casting, and the preparation process and properties of green and sintered tapes were discussed thoroughly. The effect of Si₃N₄ content on the rheological behavior of the slurries was investigated, and the results showed that the viscosity of the slurry increased with the solid loading and all the slurries exhibited shear‐thinning behavior within the entire range of shear rate. Green tapes were fabricated successfully by aqueous tape casting which have excellent properties such as uniform pore distribution, low porosity, and high bulk density. The sintered samples exhibited low shrinkage, and low dielectric constant and loss.     

Tape Casting of Lanthanum Chromite

The effects of process additives, ball milling, and solids loading were evaluated for tape casting suspensions of glycinenitrate-synthesized La_0.7Ca_0.31CrO₃ powder. An optimized formulation was obtained based on rheological characterization, electrokinetic sonic amplitude measurements, qualitative examination of green tapes, and the sintered microstructure. The tape casting formulation incorporated 66:34 methyl ethyl ketone/ethyl alcohol solvent, an aliphatic phosphate ester dispersant, and 80 wt% (35 vol%) solids. The best binder/plasticizer system was 12 wt% (15 vol%) poly(isobutyl methacrylate) and 5 wt% (6.3 vol%) benzyl butyl phthalate plasticizer (binder:plasticizer = 2.3). Cast tapes were sintered at 1300°C for 2 h, producing a bulk density of 96.2% theoretical, with linear shrinkage of 22% and an approximate grain size of 1.3 μm.     

Phase-inversion tape casting and synchrotron-radiation computed tomography analysis of porous alumina

A variant of tape casting based on the phase inversion phenomenon was adopted for fabrication of porous ceramic wafer. A slurry was prepared by dispersing alumina powder in an N-methyl-2-pyrrolidone (NMP) solution of the polymers polyethersulfone (PES) and polyvinylpyrrolidone (PVP). The slurry was cast using a doctor blade, and immersed in water to solidify the polymer solution via phase inversion. The green tape was dried and sintered at 1500 °C. The as-prepared ceramic wafer was characterized using synchrotron-radiation computed tomography (SR-CT). It was revealed that the ceramic wafer contained typical finger-like macrovoids, and the porosity resulting from these macrovoids was ~30%. The overall porosity of the wafer was 59%, as derived from the density data measured by Archimedes method in mercury. It is concluded that the phase inversion tape casting is a simple and effective method for preparation of porous ceramics.     

Tape-Casting Performance of Ethanol Slurries for the Processing of Textured PMN–PT Ceramics from Nanocrystalline Powder

The rheological behavior and tape-casting performance of ethanol-based Pb(Mg_1/3Nb_2/3)O₃–PbTiO₃ (PMN–PT) slurries is studied. A nanocrystalline powder obtained by mechanochemical activation was used. Suspensions were prepared up to solid contents of 32 vol%, significantly higher than those usually reported for nonaqueous systems. The feasibility of replacing toxic solvents commonly used for tape casting of functional ferroelectric materials, often toluene, with ethanol is demonstrated. The density, phases and microstructure of the green tapes and sintered ceramics are presented. Cube-shaped templates were successfully aligned during the tape casting for the processing of 〈001〉-textured PMN–PT ceramics by templated grain growth. An effect of the lamination of tape stacks on the template orientation is described.     

Optimization of non-aqueous tape casting of high solid loading slurry for aluminum nitride ceramic substrates

Aluminum nitride (AlN) ceramic substrates have been fabricated using non-aqueous tape casting and pressureless densification under flowing N₂ atmosphere. Considering the economic and environmental impact, a new strategy of solvent and dispersant system was adopted to prepare AlN slurries with high solid loading. According to the viscosity characteristics of AlN slurries, dispersant content was adjusted to be 0.5 wt% of AlN powder in order to optimize the rheological behavior of AlN slurries. The addition contents of binder and plasticizer were both optimized as 5 wt% of AlN powders by combining the viscosity of slurries and tensile strength of green tapes. Green AlN tapes were fabricated with an optimized tape casting process such as dry temperature. The exclusion process of organic additives was investigated by employing thermogravimetric analysis. Flat and dense AlN ceramic substrates with a relative bulk density over 99.75 % were achieved after being sintered under 1800°C for 6 hours, which had a maximum size of 110 × 110 mm. The thermal conductivity of the AlN substrate could reach 145 Wm⁻¹K⁻¹.     

Comparison of Aqueous and Non-Aqueous Tape Casting of Aluminum Nitride Substrates

A direct comparison of aqueous and non-aqueous tape casting was investigated. Aqueous and non-aqueous formulations were developed for tape casting of aluminum nitride (AlN) powder. The oxygen content of the AlN powder in aqueous ball-milling media had a slight increase, but it did not almost influence the thermal conductivity of AlN substrate. The solid loading of aqueous AlN slurry was higher than that of the non-aqueous one, but its viscosity was lower than that of non-aqueous AlN slurry. Under the same burnout program, the residual carbon content in aqueous AlN green sheet was lower than that of the non-aqueous one. The thermal conductivity of the aqueous AlN substrate sintered at 1850°C for 3 h was 138 W·(m·K)⁻¹, which was close to 142 W·(m·K)⁻¹ of the non-aqueous AlN substrate.     

Effect of CTAB as a foaming agent on the properties of alumina ceramic membranes

Alumina-ceramic membranes were prepared by gelcasting process using CTAB as a foaming agent. To increase the fineness, the starting alumina powder was milled for 1 h in a ball mill before the casting process. Particle size distribution and surface area measurements of the as-received and milled alumina powder were examined. The casted alumina membranes were sintered at 1500 °C. Sintering parameters in terms of bulk density (BD) and apparent porosity (AP) were determined by the Archimedes method. Pore size distribution of the sintered porous alumina membranes was measured using mercury porosimeter. Microstructure of sintered membranes was investigated by scanning electron microscope (SEM). Cold crushing strength (CCS) of the sintered specimens was also evaluated. The result revealed that the properties of porous ceramics such as porosity, average pore size, pore size distribution and cold crushing strength could be controlled by adjusting the preparation conditions e.g. solid loading, sintering temperature and foaming agent. The open porosity, cold crushing strength and average pore size of the alumina ceramics sintered at 1500 °C were around 58.35%, 18 MPa and178 nm, respectively.     

Aqueous tape casting of alumina using natural rubber latex binder

Eco-friendly and sustainable tape casting of alumina powder suspensions using concentrated natural rubber (poly isoprene) latex binder has been studied. The high negative zeta potential values of the aqueous alumina slurry (−53 to −72 mV) and rubber latex (−67 to −84 mV) at pH in the range of 9–11.5 enables their co-dispersion to produce tape casting slurries of solids (alumina + rubber) concentration >60 vol% with adequate flow characteristics. Drying of the slurry tape-cast on Mylar substrate is achieved within 15 min at 70 °C due to its high solid concentration. The green tapes containing 14.2 to 18.1 wt% of rubber shows tensile strength and strain at failure in the ranges of 1.85 to 1.61 and 41–254%, respectively. The flexible green tapes turn rigid by annealing at 200 °C due to the self-cross-linking of rubber chains induced by the Lewis acid sites of alumina. Thickness reduction to the extent of 20% by rolling of the green tape before annealing improves the green microstructure which results in an enhancement in sintered density from 93 to 98% of the theoretical value. However, the additional rolling and annealing steps consume extra time and energy compared to the tape casting processes using other reported binders.     

TBA-based freeze/gel casting of porous hydroxyapatite scaffolds

Porous ceramic scaffolds with a controlled “designer” pore structure have been prepared by the freeze/gel casting route using a TBA-based hydroxyapatite slurry system with 20–40 wt.% solid content. The products were characterized in terms of sintered microstructure, together with physical and mechanical properties. After sintering at 1050–1250 °C, the advantages of freeze casting and gel casting appeared in the pore structure and compressive strength of the ceramics, i.e., unidirectional aligned macro-pore channels developed by controlling the solidification direction of the TBA solvent used in the freeze casting together with small diameter (micron sized) isolated pores formed in the dense outer walls of the pore channels when processed by gel casting. The sintered porosity and pore size generally resulted in a high solid loading giving low porosity and small pore size, this leading to higher compressive strengths. The scaffolds obtained exhibited an average porosity and compressive strength in the range 41.9–79.3% and 35.1–2.7 MPa, respectively, depending on the processing conditions used.     

Effect of particle size on the shaping of ceramics by slip casting

The effect of the nanometric-ranged particle size of the starting powder through a simple and well-established shaping method, slip casting, has been studied. Several alumina suspensions with the same viscosity (but different solid content suspensions) and different particle size (11, 44, 190 and 600 nm) were prepared and shaped into a dense body. The green and sintered densities ranged between 30–67% and 63–99% of the theoretical value, respectively. These values, together with the microstructure observations reveal the effect of the solid content of the suspensions and the characteristics of the ceramic powder, leading to the determination of an optimal particle size. Based on both processability (rheological behaviour) and microstructure (density and grain size) it has been determined that particles with sizes ranging 100–300 nm are the best for preparing concentrated suspensions with low viscosity and bodies with density close to the theoretical value when using conventional pressureless sintering densification.