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Abtrag und Analyse verzunderter Stahlproben mit Laserstrahlung

机译:用激光辐射去除和分析氧化皮样品

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摘要

Laser radiation has maintained entry in his capacity as a contactless working tool into many industrial applications in the field of laser material processing like drilling or cutting of material. In the field of chemical analysis by laser-induced breakdown spectroscopy (LIBS) laser setups are used routinely e.g. for testing for mixed-up components of pipes. This work bridges the two fields of defined material ablation and chemical analysis by LIBS. Time and spatially modulated Nd:YAG laser radiation is used to ablate effectively scaled low-alloy steel surfaces and to analyse simultaneously. By using triple pulse bursts the depth penetration can be enhanced by a factor of up to 6 in comparison to single laser pulses taking the same total laser burst energy. For several elements the necessary ablation depths are estimated for a representative analysis at the scale side of the production control samples. Some elements can be analysed in the upper surface layer whereas e.g. for the element carbon a depth of at least 200 µm has to be removed. By using double pulse bursts the value of 55.2 rel.-% for the relative standard deviation of the procedure of carbon calibration at the scale side without prior material ablation can be reduced to a value of 2.8 rel.-% after removing a surface layer with a thickness of approx. 300 µm. The first time in the field of LIBS tailored crater geometries were generated by a 3D laser scanner and optimised scan strategies which lead to smaller crater debris in comparison to locally fixed laser radiation. Interactions between plasma and crater walls and with it falsified plasma compositions by scale material are reduced analysing in the middle of the produced crater. For an adequate analysis in a laser generated crater aspect ratios of smaller than 1 are to be aspired. Calibration measurements showed that the LOD values for many elements are lower than 10 µg/g up to an analysis depth of about 300 µm. With increasing number of evaluated laser pulses of up to 3000 on each sample position the LOD values are significantly improved, e.g. for Ti to 1 µg/g. Using the curve-of-growth theory conclusions can be made concerning the self-absorption of emission lines. By means of a double logarithmic plot of calibration functions the linear section can be separated from the non-linear one showing self-absorption. With calibrations in sections the analytical performance can be improved by a factor of up to 3. For the analysis of scaled steel samples a calibration method is developed using in a first step double pulse bursts. Double pulse bursts lead to an effective scale ablation and simultaneously to an analysis of elements which are already contained representatively in the upper scale layer. In the second step single laser pulses are focused onto the same sample position leading to smaller plasmas and therefore smaller self-absorption. In this way the use of several analyte lines for covering bigger concentration ranges of one element can be disclaimed. On-site measurements in a steel mill and in a hot strip rolling mill were carried out for testing the results in the industrial practice. For the test in the steel mill a laser system was built up for the combination of ablation and analysis of scaled low alloy steel samples analysing automatically the samples at different sample positions. Two methods are used for calibration. In a first step double pulse bursts and in the second step single laser pulses are taken for ablation and analysis. During the test phase the optical elements in the laser trace were not cleaned. By means of referencing and periodical recalibrations a relative standard deviation of the procedure of 2.3 rel.-% is achieved for the element Mn. The drift behaviour of the intensities can be reduced by using reference lines which lie in a similar wavelength range as the analyte line. Thereby the ambient gas emission line Ar 415.85 nm is proved to be most suitable for the analyte line Al 394.4 nm. For the on-site measurements in the hot strip rolling mill LIBS analysis at up to 520°C warm steel coils were carried out concerning the testing for mixed-up components. Seven different coils were measured by a water-cooled measuring head constructed especially for the analysis of warm coils. The setup including a 5 m long fibre optics was optimised for a high transmission of UV light in the wavelength range of about 190 nm. With this setup the accuracies of warm coils lie in a comparable range as for chilled scaled samples.
机译:激光辐射一直以其非接触式工作工具的身份进入激光材料加工领域(例如钻孔或切割)的许多工业应用。在通过激光诱导击穿光谱法(LIBS)进行化学分析的领域中,常规地使用激光装置,例如用于测试管道的混合组件。这项工作桥接了LIBS定义的材料烧蚀和化学分析的两个领域。时间和空间调制的Nd:YAG激光辐射用于烧蚀有效缩放的低合金钢表面并同时进行分析。与采用相同总激光脉冲能量的单个激光脉冲相比,通过使用三脉冲脉冲,可以将深度穿透提高多达6倍。对于几种元素,估计必要的烧蚀深度,以便在生产控制样品的比例尺一侧进行代表性分析。可以在上表面层中分析某些元素,而例如对于元素碳,必须去除至少200 µm的深度。通过使用双脉冲猝发,在不事先烧蚀的情况下,在标尺侧进行碳校准的碳校准程序的相对标准偏差的值55.2 rel .-%可以减少为去除表面涂层后的2.8 rel .-%的值。厚度约300微米通过3D激光扫描仪和优化的扫描策略,在LIBS领域首次量身定制了火山口几何形状,与局部固定的激光辐射相比,火山口碎片更小。在产生的陨石坑的中部,减少了等离子体和陨石坑壁之间的相互作用,以及通过氧化皮材料伪造的血浆成分的相互作用。为了在激光中进行充分的分析,需要产生小于1的缩孔长宽比。校准测量表明,许多元素的LOD值低于10 µg / g,直至分析深度约为300 µm。随着在每个样本位置上增加的多达3000个的评估激光脉冲数量,LOD值得到了显着改善,例如Ti的含量为1 µg / g。使用增长曲线理论,可以得出有关发射线自吸收的结论。通过校准函数的双对数图,可以将线性部分与显示自吸收的非线性部分分开。通过分段校准,可以将分析性能提高多达3倍。为了分析成比例的钢样品,第一步中使用双脉冲猝发法开发了一种校准方法。双脉冲猝发导致有效的尺度烧蚀,并且同时导致对已经代表性地包含在上部尺度层中的元素的分析。在第二步中,将单个激光脉冲聚焦在相同的样品位置上,从而导致较小的等离子体并因此导致较小的自吸收。以此方式,可以避免使用多个分析物管线来覆盖一个元素的更大浓度范围。在钢厂和热轧机中进行了现场测量,以测试工业实践中的结果。为了在钢厂中进行测试,建立了激光系统,该系统结合了烧蚀和按比例缩放的低合金钢样品分析,可以自动分析不同样品位置的样品。校准使用两种方法。在第一步中,双脉冲猝发,在第二步中,采用单个激光脉冲进行消融和分析。在测试阶段,未清洁激光走线中的光学元件。通过参考和定期重新校准,元素Mn的相对标准偏差为2.3 rel。%。通过使用与分析物线处于相似波长范围内的参考线,可以降低强度的漂移行为。因此,环境气体发射线Ar 415.85 nm被证明最适合分析物线Al 394.4 nm。为了在热轧机上进行现场测量,LIBS在高达520°C的条件下进行了热钢卷的分析,涉及混合成分的测试。通过水冷式测量头测量了七个不同的线圈,该水冷式测量头专门用于分析热线圈。优化了包括5 m长光纤的设置,以在约190 nm的波长范围内高透射紫外线。通过这种设置,热盘管的精确度可与冷氧化皮样品相媲美。

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    Vrenegor Jens;

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  • 年度 2012
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  • 正文语种 ger
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