基于高通量微区能量色散X射线荧光光谱分析的单晶高温合金枝晶结构识别与统计  

Dendritic structure recognition and statistics for single-crystal superalloys based on high-throughput micro energy dispersive X-ray fluorescence spectrometry

作　　者：刘明博 李冬玲[1,2] 倪子月 杨丽霞 沈学静[1,2] 王海舟 LIU Mingbo;LI Dongling;NI Ziyue;YANG Lixia;SHEN Xuejing;WANG Haizhou(Central Iron and Steel Research Institute Co.,Ltd.,Beijing 100081,China;NCS Testing Technology Co.,Ltd.,Beijing 100081,China)

机构地区：[1]钢铁研究总院有限公司,北京100081 [2]钢研纳克检测技术股份有限公司,北京100081

出　　处：《冶金分析》2023年第12期1-7,共7页Metallurgical Analysis

基　　金：国家重点研发计划(2021YFB3702103)。

摘　　要：为揭示铸造单晶高温合金成型过程中枝晶组织形成和生长的规律,基于自主研发的高通量微区扫描能量色散X荧光光谱分析仪(μ-EDXRF)中多元素含量分布分析功能,开发了一套枝晶结构的检测、识别、定性和定量分析方法。在经过打磨处理的样品表面选取6 mm×6 mm区域,进行步距为10μm的扫描,得到Ni、Ta、W、Re等元素的含量分布图,并观察到深浅不均的枝晶状偏析。为了使枝晶图形更加清晰、更加易于定性识别和定量分析,将各分布图进行降噪、点对点代数运算以及二值化识别等一系列图像处理操作,并参照国家标准GB/T 14999.7开发了仪器配套软件中的枝晶处理模块,自动完成枝晶组织的识别、定位、计数以及枝晶间距计算,同时利用μ-EDXRF的特点完成枝晶内部各元素偏析的定量检测。用该方法对某DD5型单晶高温合金样品进行分析,测得枝晶间距为304.2μm,与金相显微镜方法测得的数值一致,同时还得出了正负偏析点Ni、Ta、W和Re等元素含量平均值的差值超过2%的结论。In order to reveal the formation and growth laws of dendrite structure in the forming process of casting single-crystal superalloy,a set of methods for detection,recognition,qualitative and quantitative analysis of dendrite structure was developed based on the multi-element content distribution analysis function of self-developed high-throughput micro energy dispersive X-ray fluorescence spectrometer(μ-EDXRF).An area of 6 mm×6 mm was selected on the sample surface after polishing treatment for the scanning with step of 10μm.The content distribution maps of Ni,Ta,W and Re and other elements were obtained,and the uneven dendritic segregation could be observed.In order to make the dendrite pattern clearer and easier for qualitative recognition and quantitative analysis,a series of image processing operations such as denoising,point-to-point algebraic operation and binarization recognition were carried out on each distribution map.Moreover,the dendrite processing module in the matching software was developed according to GBT 14999.7,so as to automatically complete the recognition,positioning,counting of dendrite structure and dendrite spacing calculation.The quantitative detection of segregation of each element in dendrite could be also completed using the characteristic ofμ-EDXRF.The proposed method was applied for the analysis of DD5 single-crystal superalloy sample.The measured dendrite spacing was 304.2μm,which was consistent with that by metallographic microscope.It was found that the difference of average content of Ni,Ta,W and Re elements at positive and negative segregation points was more than 2%.

关 键 词：能量色散X射线荧光光谱(EDXRF) 微区分析 单晶高温合金 枝晶 元素偏析 镍 钽 钨 铼 

分 类 号：O582[理学—物理] O657.34[冶金工程—冶金物理化学] TF031