304不锈钢表面Fe_3Si型金属硅化物渗层的制备与表征
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摘要
论文采用熔融盐非电解法在AISI304不锈钢表面制备了含硅量(at.%)不同的Fe3Si型金属硅化物渗层。通过XRD、SEM、EDXS等对试样进行了表征,并分析了工艺参数对渗硅层的厚度及孔隙率的影响以及熔盐法渗硅层的形成机理等,同时对渗硅试样进行了硬度测试。另外,论文采用未经硅化处理的AISI304不锈钢作为参照,对渗硅试样在800℃、900℃下,120h的循环氧化行为进行了系统研究,并利用氧化速度常数对相关氧化动力学过程进行了理论分析。从而得到如下结果：
(1)随着渗硅剂在熔盐体系中所占比重的增多,渗硅层厚度增加且硅含量升高；提高渗硅温度则显著提高了渗硅效率；而延长渗硅时间可以提高渗硅层的致密度并细化晶粒。
(2)渗硅层是含有Ni、Cr合金元素的Fe3Si型多元过渡族金属硅化物,并且可以得到含硅量到达20at.%以上的高硅相,其仍然是D03型有序Fe3Si。而硅元素在渗层中呈均匀分布,并不存在浓度梯度,使得整个渗层的显微硬度得到显著提高,达到660HV以上。
(3)在高温循环氧化方面,Fe3Si金属间硅化物渗层表现出了较AISI 304不锈钢优越的高温抗氧化性能。Fe3Si型渗硅层在800℃、900℃下高温循环氧化120h后,其氧化动力学曲线在5h后均表现为二次抛物线型,且由于更快地生成了连续的SiO2保护膜,使得900℃下的抗氧化性能更优。
(4)实验分析证明,氧化层是以SiO2和Cr2O3为内层、Fe2O3为中间层而又以SiO2和Cr2O3为外层的多层混合氧化物结构。随着氧化的不断进行,Si的扩散成为氧化膜生长机制的主导。另外,在800℃下,氧化膜的局部存在有溃疡状孔洞,这一特征是Cr2O3在氧化过程中内部因扩散而形成的空位塌陷所致,并且伴有较多的裂纹和少量的脱皮。而900℃下的氧化层表面,只发现有少量裂纹存在。
It was prepared Fe3Si metal siliconized layer with defferent silicon content on the surface of AISI 304 stainless steel by electroless deposition used molten salt. The siliconized samples were characterized by XRD, SEM, EPMA, the paper wased analyzed affect of the process parameters to the thickness of siliconized layer and the porosity, and also the formation mechanism of siliconized layer by molten salt, at the same time, the hardness of the siliconized sample wased tested. In addition, the excellent oxidation resistance of Fe3Si based intermetallics is a predominance for using as the structural layer, so the high temperature oxidation behavior of Fe3Si metal siliconized layer was studied at 800℃、900℃for 120h with the mode of circle oxidation in present work. AISI 304 stainless steel was chosen as a reference. Besides, oxidation rate constant was used to analyze the relative materials' oxidation kinetic process theoretically. Thus we obtained following results:
(1)With the increase of the proportion of the silicon infiltration agent in molten salt, it increased the thickness of siliconized layer and silicon content. Improveing siliconized temperature significantly improved the efficiency. Extension of time could improve the density of siliconized layer and refined grain.
(2)Siliconized layer consisted of Fe3Si multivariate transitional metal silicide contained Ni, Cr alloy elements and obtained high-silicon phase which could be reached more than 20at.%. The study showed that the the high-silicon phase was still DO3-type ordered Fe3Si. Element of Si was well-distributed in the layer and there was no concentration gradient.That made the hardness of the layer significantly enhance, which could reach more than 660HV.
(3)In the high-temperature cyclic oxidation experiment, Fe3Si metal siliconized layer exhibited more excellent oxidation resistance than that of AISI 304 stainless steel. After 120h in high-temperature cyclic oxidation at 800℃and 900℃, the oxidation kinetics of the siliconized layers all showed as quadratic parabolas. As quickly generate a continuous SiO2 protective film, the high temperature resistance at 900°C was better.
(4)Experimental results showed that oxide layer made up of the mixed oxide which had multi-layer structure which consisted of the inner layer(SiO2 and Cr2O3), the middle layer(Fe2O3) and the outer layer(SiO2 and Cr2O3). With the continuous oxidation carrying on, Si diffusion bacame the dominance of growth mechanism of oxide film. In addition, at 800℃, the oxide film contained cankerous holes. This special morphology is the result of collapse of the diffusion vacancies in the Cr2O3 due to the effect of internal stress in the scales. Simultaneously, it accompanied by more cracks and a small amount of peelings. And at 900℃, on the surface of oxide film, only a lattle of cracks were found.
(1)随着渗硅剂在熔盐体系中所占比重的增多,渗硅层厚度增加且硅含量升高；提高渗硅温度则显著提高了渗硅效率；而延长渗硅时间可以提高渗硅层的致密度并细化晶粒。
(2)渗硅层是含有Ni、Cr合金元素的Fe3Si型多元过渡族金属硅化物,并且可以得到含硅量到达20at.%以上的高硅相,其仍然是D03型有序Fe3Si。而硅元素在渗层中呈均匀分布,并不存在浓度梯度,使得整个渗层的显微硬度得到显著提高,达到660HV以上。
(3)在高温循环氧化方面,Fe3Si金属间硅化物渗层表现出了较AISI 304不锈钢优越的高温抗氧化性能。Fe3Si型渗硅层在800℃、900℃下高温循环氧化120h后,其氧化动力学曲线在5h后均表现为二次抛物线型,且由于更快地生成了连续的SiO2保护膜,使得900℃下的抗氧化性能更优。
(4)实验分析证明,氧化层是以SiO2和Cr2O3为内层、Fe2O3为中间层而又以SiO2和Cr2O3为外层的多层混合氧化物结构。随着氧化的不断进行,Si的扩散成为氧化膜生长机制的主导。另外,在800℃下,氧化膜的局部存在有溃疡状孔洞,这一特征是Cr2O3在氧化过程中内部因扩散而形成的空位塌陷所致,并且伴有较多的裂纹和少量的脱皮。而900℃下的氧化层表面,只发现有少量裂纹存在。
It was prepared Fe3Si metal siliconized layer with defferent silicon content on the surface of AISI 304 stainless steel by electroless deposition used molten salt. The siliconized samples were characterized by XRD, SEM, EPMA, the paper wased analyzed affect of the process parameters to the thickness of siliconized layer and the porosity, and also the formation mechanism of siliconized layer by molten salt, at the same time, the hardness of the siliconized sample wased tested. In addition, the excellent oxidation resistance of Fe3Si based intermetallics is a predominance for using as the structural layer, so the high temperature oxidation behavior of Fe3Si metal siliconized layer was studied at 800℃、900℃for 120h with the mode of circle oxidation in present work. AISI 304 stainless steel was chosen as a reference. Besides, oxidation rate constant was used to analyze the relative materials' oxidation kinetic process theoretically. Thus we obtained following results:
(1)With the increase of the proportion of the silicon infiltration agent in molten salt, it increased the thickness of siliconized layer and silicon content. Improveing siliconized temperature significantly improved the efficiency. Extension of time could improve the density of siliconized layer and refined grain.
(2)Siliconized layer consisted of Fe3Si multivariate transitional metal silicide contained Ni, Cr alloy elements and obtained high-silicon phase which could be reached more than 20at.%. The study showed that the the high-silicon phase was still DO3-type ordered Fe3Si. Element of Si was well-distributed in the layer and there was no concentration gradient.That made the hardness of the layer significantly enhance, which could reach more than 660HV.
(3)In the high-temperature cyclic oxidation experiment, Fe3Si metal siliconized layer exhibited more excellent oxidation resistance than that of AISI 304 stainless steel. After 120h in high-temperature cyclic oxidation at 800℃and 900℃, the oxidation kinetics of the siliconized layers all showed as quadratic parabolas. As quickly generate a continuous SiO2 protective film, the high temperature resistance at 900°C was better.
(4)Experimental results showed that oxide layer made up of the mixed oxide which had multi-layer structure which consisted of the inner layer(SiO2 and Cr2O3), the middle layer(Fe2O3) and the outer layer(SiO2 and Cr2O3). With the continuous oxidation carrying on, Si diffusion bacame the dominance of growth mechanism of oxide film. In addition, at 800℃, the oxide film contained cankerous holes. This special morphology is the result of collapse of the diffusion vacancies in the Cr2O3 due to the effect of internal stress in the scales. Simultaneously, it accompanied by more cracks and a small amount of peelings. And at 900℃, on the surface of oxide film, only a lattle of cracks were found.
引文
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