Effect of varied powder processing routes on the stabilizing performance and coordination type of polyacrylate in alumina suspensions

The influence of initial pH and energy input during suspension homogenization on the stabilizing performance and coordination type of commercial available polyacrylate dispersant were studied. Additionally to widely used rheology and electroacoustic measurement techniques the alumina suspensions were analysed with centrifugal separation and in situ ATR-FTIR to study the impact of varied powder processing in detail. In contrast to zeta potential analysis and viscosity measurements only the determination of sedimentation properties by centrifugal separation shows the effect of macroscopic changes in powder processing. A combination of positively charged alumina surface and a high shear homogenization leads to the most stable suspension. Accordingly ATR-FTIR results show a correlation between improved suspension stability and inner-sphere coordination of polyacrylate. Moreover it was possible to determine an optimal pH range for inner-sphere adsorption. It can be shown that macroscopic changes in powder processing influence the coordination of dispersant and thus the suspension stability.     

Mullite coatings on ceramic substrates: Stabilisation of Al2O3–SiO2 suspensions for spray drying of composite granules suitable for reactive plasma spraying

The present work deals with the preparation of stable alumina + silica suspensions with high solid loading for the production of spray-dried composite powders. These composite powders are to be used for reactive plasma spraying whereby the formation of mullite and the coating on a ceramic substrate are achieved in a single step process. Electrostatic stabilisation of alumina and silica suspensions has been studied as a function of pH. Silica suspensions are most stable at basic pH whereas alumina suspensions are stable at acidic pH. The addition of ammonium polymethacrylate (APMA) makes it possible to stabilise alumina and prepare a stable 50 wt% alumina + silica suspension at pH 10. The optimum amounts of dispersant and binder have been determined by zeta potential, viscosity and sedimentation measurements. Spray drying of the suspension yields composite powders whose morphology, size distribution and flowability have been characterized before realizing reactive plasma spraying tests.     

Dispersion and Setting of Powder Suspensions in Concentrated Aqueous Urea Solutions for the Preparation of Porous Alumina Ceramics with Aligned Pores

Highly concentrated alumina powder suspensions have been prepared in aqueous urea solutions of concentrations in the range 200–360 g/100 mL using an ammonium poly(acrylate) dispersant at 80°C. The dispersant concentration for the suspension viscosity minimum in the urea solutions is higher than that in water due to the higher processing temperature. The urea solutions having higher dielectric constant than that of water offer higher interparticle potential that resulted in better dispersion of the powder as evidenced from the lower viscosity and yield stress of the suspensions. The decrease in temperature increased the suspension viscosity and the suspension formed a strong gel when cooled to room temperature due to the crystallization of urea. The minimum urea solution concentration for a 55 vol% alumina suspension to form a dimensionally stable gel is 240 g/100 mL. The compressive strength and Young's modulus of the gels increased with the increase in urea solution concentration. The alumina ceramics prepared by the urea removal followed by sintering at 1500°C had porosity in the range 28–36 vol% with the rectangular rod‐shaped aligned pores.     

Ink-Jet Printing of Wax-Based Alumina Suspensions

Suspensions of fine alumina powder in a paraffin wax have been successfully formulated with viscosity values sufficiently low to allow ink-jet printing using a commercial printer. A commercial-grade paraffin wax, with stearylamine and a polyester, were used as the dispersant system. Suspensions with powder loadings up to 40 vol% were passed through the ink-jet printer head. Unfired ceramic bodies with a feature size of <100 μm have been successfully fabricated with waxes that had a powder loading of 30 vol%. The influence of suspension fluid properties on the ink-jet printing process has been studied, and the importance of the acoustic resonance within the ink-jet printing apparatus has been demonstrated.     

Ascorbic acid as a dispersant for concentrated alumina nanopowder suspensions

The stabilization of concentrated nanopowder suspensions is crucial for many industrial applications. Yet, controlling the suspension viscosity is challenging for nanopowder suspension systems. In this study, we examined the adsorption of l-ascorbic acid (Vitamin C) on alumina surfaces and the related reduction in viscosity of the suspensions. Interactions between the ascorbic acid and the alumina surface were investigated by in situ ATR-FTIR and zeta potential measurements. It was shown that ascorbic acid forms complexes with the alumina surface through ligand exchange mechanisms. The optimum concentration of ascorbic acid for minimum suspension viscosity was determined. The maximum achievable solids content could be increased to around 0.35 by the addition of only 1.0 wt.% of dry powder ascorbic acid. Because ascorbic acid is easy to use, inexpensive, and a non-toxic organic additive, it has great potential to be used as a dispersant in a variety of industrial applications, from dilute to concentrated systems of intermediates or products.     

悬浮聚合用HAP／SDBS无机分散体系的作用机理

研究了ＨＡＰ粉末的沉降特性与生成过程，考察了ＨＡＰ粉末和不同表面活性剂配合在苯乙烯单体分散液中的吸附特性，同时研究了ＨＡＰ粉末复合不同表面活性剂的无机分散体系用于苯乙烯单体悬浮聚合时的聚合稳定性。对ＨＡＰ／ＳＤＢＳ无机分散体系用于悬浮聚合时的分散作用机理进行了探讨。简化了用于苯乙烯悬浮聚合用ＨＡＰ的制备方法：取消缓冲体系，缩短陈化时间，室温制备。且制备的分散剂用于聚合时为常量的１／５。     

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

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.     

Al2O3表面化学特性的研究

通过测量粉体在水溶液中的Ｚｅｔａ电位和颗粒大小,探讨了引入不同的分散剂如聚甲基丙烯酸氨（Ｄａｒｖａｎ Ｃ）、聚乙烯亚胺（ＰＥＩ）及 柠檬酸氨（ＤＡＣ）时Ａｌ２Ｏ３粉体表面带电状况及颗粒分散状况的变化。结果表明,在不同分散条件下的水溶液中,Ａｌ２Ｏ３表面的荷电会有非常显著的变化,Ａｌ２Ｏ３粉体的等电点会发生明显的偏移,并且在远离等电点处,Ａｌ２Ｏ３粉体呈单分散状态,在靠近等电点处,Ａｌ２Ｏ３呈现不同     

Preparation of α-Alumina Platelets by Laser Scanning

A laser scanning with gas jet process was developed to prepare alumina platelets from an alumina powder. When the carbon-dioxide laser scanned the alumina powdery coatings prepared using an electrospraying technique, the alumina particles were heated to a melting state. The coaxial gas ejection force pushed the melting particles to obtain tabular shape grains that recrystallized into alumina platelets in the subsequent rapid-cool solidification. The phase and morphologies of powder bed were characterized by XRD and SEM. Results show that only α-alumina platelets were formed in the scanning process and the average edge length and thickness is 10 μm and 1–2 μm, respectively. Laser processing parameters such as laser energy density, scanning speed, and gas pressure were expected to play a vital role in the melting-crystallization-solidification process for obtaining platelike grains from powder beds. The preliminary experiment showed that the laser-scanning technique could be an effective means of tailoring the morphologies of particles to meet application requirements.     

Spontaneous manufacturing: alumina 128-well plates made by droplet drying

Abstract

The radial flow inherent in the drying of a sessile drop has inspired the idea of preparing ceramic microwells from deposition of droplets of ceramic suspension. In this way, the shape of each well is created spontaneously without the need for a forming operation. A rectangular plate of alumina powder was made by conventional compaction and cylindrical discs were printed and sintered on its upper surface. A suspension containing the same alumina powder was printed on these discs to form droplets which were left to dry. As they did so, the powder spontaneously assembled at the periphery to form microwells. After sintering, a 128-well plate was prepared which is suitable for high temperature combinatorial experiments.     

PAA-NH_4对氧化铝悬浮液沉降性能的研究

采用PAA-NH4作为分散剂制备了超细氧化铝悬浮液,通过沉降实验观察了PAA-NH4的添加量、pH值对α-A12O3低固含量悬浮液的沉降性能的影响,并用Zeta电位仪测定了不同pH值条件下稀固相含量悬浮液的Zeta电位;同时对烧结坯体进行了微观分析.结果表明:分散剂PM-NH4的最佳用量为1.0%左右,最佳pH值为9;对添加PAA-NH4前后的稀悬浮液Zeta电位进行了测定,发现等电势点左移,Zeta电位的绝对值变化显著.添加PAA-Nh4后,pH值的变化对悬浮液的沉降性能和Zeta电位影响很大.     

Preparation of alumina by aqueous gelcasting

The alumina ceramic was prepared by aqueous gelcasting. The effects of zeta potentials, solid loading, dispersant content and milling time on the alumina suspension were studied systematically. The dispersant content has remarkable effects on the viscosity of the suspension. The appropriate dispersant concentration for alumina aqueous slurry with the solid loading of 55 vol.% is 0.6 wt.%. It can be seen that all suspensions (50–56 vol.% solid loading) exhibited a shear-thinning behavior and relatively low viscosity, which was suitable for casting. The degree of shear thinning and the viscosity at high shear rates increased with increasing volume fraction of solid. As the milling time prolongs, viscosity of the suspension decreases first, then the plateau appears and the average diameter keeps changeless. When the milling time was shorter than 20 h, the viscosity of slurries decreased gradually as the time of milling increased. After 20 h milling, the viscosity of the slurry tended to be consistent. Therefore, the ball milling time should be equal to or more than 20 h to obtain a stable suspension at equilibrium. The time available for casting the slurry (idle time) can be controlled by the amounts of initiator and catalyst added to the slurry as well as by the processing temperature. Micrograph of the gelcast green body was homogeneous.     

PAA—NH4对氧化铝悬浮液沉降性生能的研究

采用PAA—NH4作为分散剂制备了超细氧化铝悬桴液,通过沉降实验观察了PAA-NH4的添加量、pH值对α—Al2O3低固含量悬浮液的沉降性能的影响,并用Zeta电位仪测定了不同pH值条件下稀固相含量悬浮液的Zeta电位;同时对烧结坯体进行了微观分析。结果表明：分散剂PAA—NH4的最佳用量为1．0％左右,最佳pH值为9;对添加PAA—NH4前后的稀悬浮液Zeta电位进行了测定,发现等电势点左移,Zeta电位的绝对值变化显著。添加PAA-NH4后,pH值的变化对悬浮液的沉降性能和Zeta电位影响很大。     

影响氮化硅浆料流变特性的因素

通过对影响氮化硅浆料流变性因素的研究发现：不同的氮化硅粉体具有不同的等电点（ｉｓｏｅｌｅｃｔｒｉｃ ｐｏｉｎｇ,简称ＩＥＰ）。分散剂的引入明显改善浆料的流动性。对于粉体Ａ,当分散剂用量达１．２ｗｔ％时浆料具有最佳的流动性。颗粒尺寸及其形貌对浆料的流动性均有较大的影响：颗粒尺寸越大,颗粒形貌越不规则,浆料的流动性就越差。     

ZTA复相陶瓷凝胶注模成形工艺的研究

本文研究了ＺｒＯ２（３Ｙ）－Ａｌ２Ｏ３复相陶瓷的凝胶注模成形工艺,着重研究了低粘度高固相体积分数浓悬浮体的制备。     

Influence of a few important parameters on the rheological behaviour of silicon carbide nanoparticles dispersed aqueous suspension

In this study, investigations have been carried out on the effect of a few important parameters such as molecular weight and concentration of dispersant (polyethyleneimine) as well as that of pH on the rheological behaviour of aqueous suspension comprising silicon carbide (SiC) nanoparticles. In addition to this, the effect of particle size and addition of finer SiC particles on the rheological behaviour of SiC suspension have been examined. It is observed that viscosity of suspension increases with the increase in molecular weight of dispersant and decreases as the concentration of dispersant increases. Further, it is noticed that viscosity of the suspension progressively increases below the pH ≈?7.6 and above the pH ≈?9.3, indicating that minimum viscosity i.e. maximum stabilization of suspension is obtained within the pH range of ≈ 7.6–9.3. It has been observed that variation of SiC particle size from submicrometer to nanometer range and addition of nanometric SiC powder in SiC suspension containing coarser particles increase the viscosity significantly.     

Direct coagulation casting of YSZ powder suspensions using MgO as coagulating agent

Direct coagulation casting (DCC) of aqueous 8 wt% yttria stabilized zirconia (YSZ) powder suspensions prepared using ammonium poly(acrylate) dispersant has been studied using MgO as coagulating agent. Small amount (<0.1 wt% based on YSZ) of MgO powder dispersed in the YSZ powder suspension at ∼5 °C set the suspension in to stiff wet-coagulated body when exposed to room temperature (30 °C) due to the reaction between ammonium poly(acrylate) and MgO. MgO concentration equivalent to react with dispersant did not coagulate the YSZ powder suspension though it precipitate the whole ammonium poly(acrylate) dispersant as Mg-poly(acrylate). This is because of the ability of the YSZ powder to disperse in water at alkaline pH (∼9.5) without any dispersant by electrostatic mechanism. The YSZ powder suspensions form stiff coagulated bodies at MgO concentration double or more of the equivalent amount required for reacting with the dispersant. Setting of the YSZ powder suspension is due to the heterocoagulation of the YSZ particles and MgO particles added in excess of the equivalent amount to react with the dispersant, having opposite surface charges. The wet-coagulated body showed relatively high compressive yield strength (155 kPa) and Young’s modulus (3.1 MPa). The green bodies prepared by humidity controlled drying of the wet-coagulated bodies sintered to >98% TD at 1550 °C.     

The influence of solid loading in suspensions of a submicrometric alumina powder on green and sintered pressure filtrated samples

The present work deals with preparation of stable suspensions of a submicrometre alumina powder with different contents of solid for pressure filtration. The optimum dispersant content (2.2 wt.% of Darvan C-N) was determined by sedimentation tests and viscosity measurements. By modification of the solid loading and dispersant content two kinds of aggregation were observed. One type of aggregates is related to the use of excessive solid loading in suspension. In samples prepared from these suspensions only minor effect on sintered microstructure was observed, which increased with increasing volume fraction of hard aggregates. In case of excess dispersant addition weak aggregates formed as the result of depletion flocculation. Weak aggregates had stronger negative effect on green microstructure, with consequent negative impact on sinterability.     

Fabrication of textured alumina by magnetic alignment via gelcasting based on low-toxic system

The controlled development of texture in ceramics allows to improve some electrical, piezoelectric and mechanical properties of advanced ceramics materials by tailoring the microstructure. A highly textured microstructure of undoped dense alumina was attained by applying a novel combination of gelcasting techniques with magnetic alignment followed by sintering. A newly synthesized low-toxic acrylic monomer based on galactose was introduced to the gelcasting procedure. Thermal analysis of the gelcast has been performed to examine decomposition process of the new binder and match appropriate sintering rate. The effectiveness of the proposed procedure has been related to rheological properties of the suspension by clarifying the influence of the powder and the dispersant content. It has been also related to the idle time of polymerization by clarifying the influence of the initiator content. The new method is compared to slip casting in high magnetic field that has been used widely so far.     

Effects of dispersant concentration and pH on properties of lead zirconate titanate aqueous suspension

Lead zirconate titanate (PZT) aqueous suspensions were prepared at 60 wt.% solids loading using a commercial ammonium polyacrylate (APA) dispersant. Effects of the dispersant concentration on rheological behavior, dispersion and stability of PZT aqueous suspensions were investigated by means of zeta potential, viscosity and sedimentation height measurements. The results showed that, under suitable conditions, APA dispersant promoted particle dispersion and stabilization in PZT aqueous suspensions. For 60 wt.% solids loading suspensions, the dispersant concentration yielding the lowest viscosity was 0.5 wt.% based on PZT powder dried weight basis. Effects of pH on particle dispersion in the suspensions prepared with APA were studied by laser light scattering technique and scanning electron microscopy. The results showed an improvement in particle dispersion for the alkaline condition, which led to relatively low viscosity and highly stable suspension. Possible particle stabilization mechanisms at various pHs were discussed based on dissociation of the dispersant in water, polymer conformation and adsorption behavior of the dispersant on the particle surface.