| XRF is abbreviation of X-ray fluorescence spectrometry analysis.According to different analysis principles,it can be divided into two categories:wavelength dispersive X-ray fluorescence analysis(WDXRF)and energy dispersive X-ray fluorescence analysis(EDXRF).X-ray fluorescence spectrometry analysis of nickel-based alloys does not have the corresponding national standards and specifications,the influence factors are different under different alloy matrix composition,different equipment environment and different experimental parameters,and the XRF analysis results are quite different.At the same time,the chemical composition of modern nickel-based alloys is very complex,and the saturation of alloys is very high.It puts forward higher requirements for the accuracy and accuracy of chemical composition analysis,and poses new challenges to the on-site analysis of enterprises.In this paper,According to Axios MAXwavelength dispersive sequential X-ray fluorescence spectrometer,the wavelength dispersion X-ray fluorescence analysis of nickel-based alloys is studied.The curve correction and analysis parameters of nickel-based alloy determination process were studied by theoretical research,experimental research and simulation calculation,so as to obtain appropriate method parameters and establish a method which can rapidly and effectively analyze Mn,Cr,Ni,Si,Cu,W,V,Ti,Co,Mo,Nb,Al,Fe and P in nickel-based alloy.The main achievements are as follows:1.The process principle of X-ray fluorescence characteristic line generation was studied,and the optimal selection of analytical characteristic line for elements in nickel-based alloys was confirmed by theoretical calculation.That is to say,L?spectral line is used for tungsten element and K?spectral line is used for other main elements.2.The diffraction principle of X-ray fluorescence characteristic lines is studied,and the selection of spectrophotometric crystals in the process of element analysis is confirmed by combining the structure of the spectrophotometric detection system of Axios MAXwavelength dispersion sequential X-ray fluorescence spectrometer.The main spectroscopic crystals used are Li F200,Li F220,PE002 and Ge111.After confirming the spectroscopic crystals,the optimum diffraction angle of each element in the analysis process was confirmed by peak intensity scanning experiment.3.Experiments on excitation conditions of X-ray tube were carried out.The peak intensity and peak-to-back ratio of each element under different excitation conditions were studied.The excitation rules of characteristic spectral lines of different elements were studied.The optimum excitation conditions of each element in the process of X-ray fluorescence analysis were confirmed.The results show that heavy elements with large atomic number are more suitable for high voltage excitation,and light elements with small atomic number are more suitable for low voltage and high current excitation.4.The overlapping interference of spectral lines and matrix absorption enhancement effect are studied.The analytical curve is drawn,the curve correction model is established,and the curve interference correction fitting calculation is carried out.The correction curve K value is between 0.01020-0.04904,RMS value is between 0.00422-0.30756.The curve after fitting and correction has good linearity,which basically solves the disadvantageous influence of overlapping interference and matrix effect on the accuracy of analytical results.5.The precision and accuracy experiments of the analysis method show that the relative standard deviation and relative error are small,and the reliability of the analysis results is good.The relative standard deviation ranges from 0.06%to 13.22%,and the average relative error ranges from 0.17%to 7.12%.The precision and accuracy experiments of the analysis method show that the relative standard deviation and relative error are small,and the reliability of the analysis results is good. |
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