RESUMO
Environmental factors include sample temperature, ambient gas composition, and pressure, which have a significant impact on the accuracy and stability of the analysis results of laser-induced breakdown spectroscopy (LIBS). In this study, a method for simultaneously correcting the influence of several environmental factors is proposed. When the calibration and application environment are different, only one sample is needed to be measured in the application environment to correct the influence of environmental factors, so that the calibration model can obtain good analytical accuracy in this environment. When using one to four samples to correct the influence of environmental factors, the application of the calibration models constructed under solid-state conditions at atmosphere pressure to analyze seven elements in molten alloys in vacuum demonstrated the average root mean square error of prediction (RMSEP) of 0.57%, 0.51%, 0.41%, and 0.30% respectively. The accuracy of using only one sample to correct the influence of environmental factors was much higher than using two samples to establish calibration models in the application environment. This proved the effectiveness of the developed method for reducing the difficulty and cost of calibration in the metallurgical processes.
RESUMO
An active Q-switching light-emitting diode (LED)-pumped laser is demonstrated by Nd:YLF crystal with acousto-optic modulation for the first time. The spectrum-band pump characteristic is grasped to describe the essential difference between an LED pump and single-absorption-peak matching of laser-diode pump or no matching of lamp pump. An effective absorption spectrum concept is proposed to characterize the absorption features of the gain material with LED-band pumping. According to this new theory, a flat-top beam profile is designed for pumping Nd:YLF crystal with only a 14 W/cm2 peak power, resulting in 165 µJ output energy at 1047 nm. More importantly, by using the acousto-optic Q-switching technique, this LED-pumped Nd:YLF laser has successfully realized a TEM00 mode output with a pulse energy of 10.6 µJ and a pulse width of 452 ns.
RESUMO
Vacuum induction melting is a popular method for refining high purity metal and alloys. Traditionally, standard process control in metallurgy involves several steps, include drawing samples, cooling, cutting, transport to the laboratory, and analysis. The whole analysis process requires more than 30 minutes, which hinders on-line process control. Laser-induced breakdown spectroscopy is an excellent on-line analysis method that can satisfy the requirements of vacuum induction melting because it is fast and noncontact and does not require sample preparation. The experimental facility uses a lamp-pumped Q-switched laser to ablate melted liquid steel with an output energy of 80 mJ, a frequency of 5 Hz, a FWHM pulse width of 20 ns, and a working wavelength of 1,064 nm. A multi-channel linear charge coupled device (CCD) spectrometer is used to measure the emission spectrum in real time, with a spectral range from 190 to 600 nm and a resolution of 0.06 nm at a wavelength of 200 nm. The protocol includes several steps: standard alloy sample preparation and an ingredient test, smelting of standard samples and determination of the laser breakdown spectrum, and construction of the elements concentration quantitative analysis curve of each element. To realize the concentration analysis of unknown samples, the spectrum of a sample also needs to be measured and disposed with the same process. The composition of all main elements in the melted alloy can be quantitatively analyzed with an internal standard method. The calibration curve shows that the limit of detection of most metal elements ranges from 20-250 ppm. The concentration of elements, such as Ti, Mo, Nb, V, and Cu, can be lower than 100 ppm, and the concentrations of Cr, Al, Co, Fe, Mn, C, and Si range from 100-200 ppm. The R2 of some calibration curves can exceed 0.94.