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Structural Characterization and Corrosion Behavior of Stainless Steel Coated With Sol-Gel Titania

机译:溶胶-凝胶二氧化钛涂层不锈钢的结构表征和腐蚀行为

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Sol-gel titania films were prepared from hydrolysis and condensation of titanium (IV) isopropoxide. Diethanolamine was used as chelant agent in titania synthesis. 316L stainless steel substrates were dip-coated at three different withdrawal speeds (6, 30, and 60 mm/min) and heated up to 400℃. Thermo-gravimetry and differential thermal analyses of the titania gel solution evinced a continuous mass loss for temperatures up to 800℃. The transition of anatase to the rutile phase begins at 610-650℃, being the rutile transformation completed at 900℃. The thicknesses of the films were determined as a function of the heat treatment and withdrawal speed. It was observed that their thicknesses varied from 130 to 770 nm. Scanning electron microscopy images of the composites revealed the glass-like microstructure of the films. The obtained sol-gel films were also characterized by energy dispersive spectroscopy. The chemical evolution of the films as a function of the heating temperature was evaluated by Fourier transform infrared spectroscopy (specular reflectance method). After performing the adhesion tests, the adherence of the titania films to the stainless steel substrate was excellent, rated 5B according to ASTM 3359. The hardness of the ceramic films obtained was measured by the Knoop microindentation hardness test with a 10 g load. We observed that the titania film became harder than the steel substrate when it was heated above 400℃. The corrosion rates of the titania/steel composites, determined from potentiodynamic curves, were two orders of magnitude lower than that of the bare stainless steel. The presence of the sol-gel titania film contributed to the increase of the corrosion potential in ca. 650 mV and the passivation potential in ca. 720 mV.
机译:溶胶-凝胶二氧化钛薄膜是由异丙醇钛(IV)的水解和缩合制备的。二乙醇胺在二氧化钛合成中用作螯合剂。 316L不锈钢基材以三种不同的退出速度(6、30和60 mm / min)浸涂,并加热到400℃。二氧化钛凝胶溶液的热重分析和差热分析表明,在高达800℃的温度下,质量持续损失。锐钛矿到金红石相的转变始于610-650℃,是金红石的转变在900℃完成。确定膜的厚度作为热处理和抽出速度的函数。观察到它们的厚度在130至770nm之间变化。复合材料的扫描电子显微镜图像显示了膜的玻璃状微观结构。所获得的溶胶-凝胶膜还通过能量色散光谱法表征。通过傅立叶变换红外光谱法(镜面反射法)评估了膜的化学演化与加热温度的关系。进行粘合试验后,二氧化钛膜对不锈钢基材的粘合性极好,根据ASTM 3359评定为5B。通过努氏显微压痕硬度试验在10 g载荷下测量所得陶瓷膜的硬度。我们观察到,当加热到400℃以上时,二氧化钛膜变得比钢基底硬。由电位动力学曲线确定的二氧化钛/钢复合材料的腐蚀速率比裸不锈钢低两个数量级。溶胶-凝胶二氧化钛膜的存在有助于增加约200毫米的腐蚀电位。 650 mV,钝化电势约为720毫伏。

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