A new method for detection and assessment of inclusions in clean steels based on laser ablation and ICP mass spectrometry has been developed. Samples were subjected to UV laser ablation (Nd Yag) and ion intensities of elements of interest were monitored on a time-resolved basis. Lasers exhibiting both gaussian and flat-top intensity beam distributions were used. Analytical response for inclusion and matrix elements as a function of laser ablation parameters was studied and procedures were developed for rapid inclusion characterisation and elemental mapping. Main inclusion types identified in clean steels were Mn-S, Mg-Al and Mg-Al-Ca-Ti-Si. Results indicate the considerable analytical potential for the laser ablation technique in a production environment.KEY WORDS: clean steels; inclusions; mapping laser ablation; ICP mass spectrometry.a versatile microanalytical technique and is analogous to the SSE method in that elemental analysis is based on direct spectral observation of the plasma discharge. LIBS has yet to be fully exploited for characterisation of inclusions in clean steels but the potential is considerable given its success as a microanalytical tool [8][9][10][11] for spatially resolved measurement and depth profiling. 10,[12][13][14] Progress in the use of LIBS for inclusion measurement has recently been elaborated by Noll et al. 15) and Laserna et al.
16)Laser ablation in combination with ICP emission or ICP mass spectrometry constitutes an important bulk and microanalysis tool as evidenced by an extensive literature. [17][18][19] Relative to the LIBS approach a major advantage of the laser-ICP combination is the improved measurement sensitivity particularly for ICP-MS detection where the current state of the art is at the ng/g level. The high detection sensitivity combined with good spatial measurement capability has been exploited in geological investigations including the characterisation of fluid inclusions [20][21][22] and for zonation studies in minerals. [23][24][25] The aim of this research was to evaluate the potential of the LA-ICP-MS method for steel cleanness assessment. The effects of key parameters, i.e. laser energy, frequency, spot size, and rate of sample translation on signal response have been investigated using both gaussian and flat top beam intensity distribution profiles. The approach permits rapid identification of elements present in inclusions and gives new information related to the spatial distribution of inclusions in samples.
Experimental
MaterialsA glass standard reference material (SRM 612, NIST, Gaithersburg, MD) was used for initial instrument set-up (daily basis) and in-house research materials previously characterised by optical metallography were used in method development.
InstrumentationLaser ablation was performed using Nd Yag lasers (LSX-100 and LSX-200, frequency quadrupoled; CETAC Technologies, Omaha) interfaced to an ICP mass spectrometer (Agilent Technologies, HP 4500). The main difference in the two laser systems was that the LSX-100 exhibits a gaussian ...