Effect of pH, milling time, and Isobam content on porous silicon nitride ceramics prepared by gel casting

Hailing Yang , Zhi Wang , Mengyong Sun , Fei Chen , Jun Ji , Sique Chen , Yingying Chen , Deli Ma , Zhenyu Zhang , Baocai Pan , Yulin Wei , Qinggang Li
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Abstract

As a non-toxic copolymer of isobutylene and maleic anhydride, Isobam is successfully used as a dispersant and a gelling agent for fabricating porous Si3N4 ceramics by gel casting. The dispersity and rheological properties of the Si3N4 slurry are influenced by the pH, milling time, and Isobam content which varies from 0.1 ​wt.% to 0.6 ​wt.%, and these factors are investigated. The slurry with 40 ​vol.% solid content and milled for 4 ​h has a high zeta potential at pH 12 (adjusted by Tetramethyl ammonium hydroxide (TMAH)), which means that the particles are well dispersed. The mechanisms of TMAH are electrostatic repulsion and steric hindrance. The viscosity of the slurry increases with the increase of Isobam content. After pressureless sintering at 1700 ​°C for 2 ​h, a uniform unique interlocking microstructure of rod-like β-Si3N4 grains is observed, which may improve the flexural strength of the ceramics by intergranular fracture and particle pullout of β-Si3N4 grains. The density and porosity of the samples fluctuate negligibly with the increase of Isobam content, and the Si3N4 ceramic with 0.1 ​wt.% Isobam exhibits the highest bending strength of 251.6 ​MPa among all samples.

Abstract Image

pH、研磨时间和异硫胺含量对凝胶铸造多孔氮化硅陶瓷的影响
Isobam作为异丁烯和马来酸酐的无毒共聚物,成功地用作分散剂和胶凝剂,通过凝胶浇铸制备了多孔Si3N4陶瓷。Si3N4浆料的分散性和流变性受到pH值、研磨时间和Isobam含量的影响,Isobam的含量从0.1变化​重量%至0.6​并对这些因素进行了研究。浆液含40​固体含量vol.%并研磨4​h在pH 12下具有高ζ电位(通过氢氧化四甲基铵(TMAH)调节),这意味着颗粒被良好分散。TMAH的作用机制是静电排斥和空间位阻。浆料的粘度随着异丁酰胺含量的增加而增加。1700无压烧结后​2°C​h、 观察到均匀独特的棒状β-Si3N4晶粒互锁微观结构,这可能通过β-Si3O4晶粒的晶间断裂和颗粒拔出来提高陶瓷的抗弯强度。随着Isobam含量的增加,样品的密度和孔隙率的波动可以忽略不计,而Si3N4陶瓷的密度和孔隙度为0.1​wt.%Isobam表现出251.6的最高弯曲强度​MPa。
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