Analysis Of Elements In Metal Oxide Nanofilms Based With LIBS Technology

With the rapid development of semiconductor thin film materials,functional metal oxide nano films have been widely used in many fields.As a commonly used preparation method of thin film materials,magnetron sputtering method is affected by operating parameters,which tends to change the ratio of components of the thin film,resulting in the corresponding differences in the photoelectric properties of the thin film.During the preparation process of the functional layer of(Cu(In_1-x,Ga _x)Se₂,CIGS)thin film solar cell and the new wide band gap semiconductor transparent conductive thin film material Al-In-Sn-O(AITO),the concentration ratio of Ga/(In+Ga),Cu/(In+Ga),Al/(Al+In+Sn)and Sn/(Al+In+Sn)has a great influence on the photoelectric properties of the thin film.Some commonly used elemental analysis methods have more or less some deficiencies,which are difficult to meet the requirements of real-time,rapid and simple operation.Laser-Induced Breakdown Spectroscopy(Laser-Induced Breakdown Spectroscopy,LIBS)technology by collecting pulse produced by the interaction between laser and material to be detected transient plasma,plasma emission spectrum analysis of the characteristic spectral lines,for detecting treated material element composition and concentration analysis techniques.LIBS technology,as an emerging component analysis technology,has been widely used in many fields due to its advantages of fast real-time,no sample pretreatment,multi-element simultaneous analysis,micro-loss and so on.In view of the traditional analysis method in the analysis of functional metal oxide thin film materials of some deficiencies,this paper studied the metal oxide nanometer thin film based with the technology of LIBS in element analysis method.Nanosecond laser-induced breakdown spectroscopy(Nanosecond-LIBS,NS-LIBS)technology has been used for preliminary experimental exploration of CIGS thin film,and the related parameters of NS-LIBS experimental device have been optimized,samples of CIGS films were prepared by magnetron sputtering under different sputtering conditions.The spectral data of the samples were compared with the composition ratio,transmittance,band gap width and so on,the feasibility of this experimental method is verified,and a direct relationship between the photoelectric properties of CIGS thin films and the analytical spectra of the target elements is established in this paper.The depth profile of multilayer CIGS films was analyzed by Picosecond-LIBS(PS-LIBS)technique,and the evolution trend of line intensity under different laser ablation times is obtained.A rapid LIBS microanalysis of AITO films using PS-LIBS produced ablation pits of about 50 microns in diameter,and a quantitative analysis study of the concentration ratio of key elements Al/(Al+In+Sn),the results show that the linear fitting is more than 0.99,the plasma temperature is 5063 K and the electron density is 4.6×10¹⁶ cm^-3 by Boltzmann diagonal method.Through the accumulation of a large number of experimental data,the comprehensive quantitative analysis of the target element concentration ratio of CIGS and AITO samples was carried out respectively.The calibration curves under single sputtering condition were fused to obtain the comprehensive calibration curves under multivariable conditions.The accuracy of the comprehensive calibration curves of several element concentration ratios was tested by using two samples prepared under arbitrary conditions,the results show that the error of the two methods are less than 4.5%.