单脉冲和再加热正交双脉冲激光诱导击穿光谱对比研究

为了提高激光诱导击穿光谱技术(LIBS)的检测灵敏度和辐射光谱特性,采用再加热正交双脉冲结构对样品中的4种元素Fe,Pb,Ca和Mg以及含有不同浓度重金属元素Cr的土壤样品进行分析。研究了4条特征谱线FeⅠ：404.581 nm,PbⅠ：405.78 nm,CaⅠ：422.67 nm和MgⅠ：518.361 nm的光谱强度和信背比随两激光脉冲之间时间间隔的变化关系,获得了两激光脉冲之间最佳的时间间隔为1.0 μs。在单脉冲和双脉冲条件下,得到了4条特征谱线FeⅠ：404.581 nm,PbⅠ：405.78 nm,CaⅠ：422.67 nm和MgⅠ：518.361 nm光谱强度的增强倍数分别为2.23,2.31,2.42和2.10;分析了特征谱线FeⅠ：404.581 nm和CaⅠ：422.67 nm谱线强度随时间的演化特性以及4条特征谱线信背比随光谱采集延时的变化关系,双脉冲能有效延长光谱强度的衰减时间以及提高特征谱线的信背比;比较分析了等离子体温度和电子密度随时间的演化特性,在双脉冲条件下,等离子体温度最大升高了730 K,电子密度最大增加了1.8×1016 cm-3。单脉冲和双脉冲条件下获得重金属元素Cr的检测限分别为38和20 μg·g-1,再加热正交双脉冲技术使元素检测限下降近2倍。以上结果表明：再加热正交双脉冲能有效地提升LIBS技术的检测灵敏度和光谱特性,为进一步降低元素的检测限提供了有效的方法。     

LIBS技术对羊毛脂复合物中重金属元素的成分分析

利用激光诱导击穿光谱技术对市面上某型号口红的羊毛脂复合物中重金属元素进行分析,使用波长为532nm的激光在口红表面击穿诱导高温等离子体,通过对MCP增益、延迟、门宽三个参数的优化来获得最佳光谱.由发射光谱线的强度计算等离子体的电子温度,研究了激光诱导等离子体的电子温度随时间演化的特性.     

磁约束飞秒激光诱导铜等离子体特性研究

建立磁约束飞秒激光诱导铜等离子体辐射光谱采集系统,通过发射光谱法分析磁约束效应对飞秒激光诱导铜等离子体特性的影响.在强度为0.67T的稳磁场约束下,等离子体辐射连续谱和分立谱均有增强,分立谱线增强更显著;铜原子上能级越高,其辐射的原子谱线增强因子越大,具有最高上能级的Cu I 507.6nm增强因子最大,为2.8;等离子体铜原子谱线持续时间明显延长,在等离子体演化初期,谱线增强显著,在较大延时,谱线增强迅速减弱;等离子体电子温度和电子密度均有提高.     

飞秒激光多脉冲烧蚀镍钛合金的数值模拟

为了研究飞秒激光多脉冲累积效应对镍钛合金材料的影响,通过考虑多脉冲之间的时间间隔改写激光光源项,利用改进的双温模型,采用有限差分法,对飞秒激光三脉冲烧蚀镍钛合金的温度场分布进行数值模拟,得到了电子和晶格温度随时间和烧蚀深度的演化规律.分析了多脉冲累积效应的内在机理;讨论了三脉冲条件下不同参量对电子和晶格温度的影响.结果表明:镍钛合金在飞秒激光三脉冲的作用下,电子有3个递增的峰值温度,相比单脉冲的作用,三脉冲使电子和晶格温度明显升高;多脉冲的时间间隔直接影响多脉冲的累积效应;脉冲宽度影响电子的峰值温度和达到峰值温度所用的时间;激光能量密度影响电子和晶格的温度;电声耦合常量对电子与晶格的耦合时间和电子晶格的平衡温度也有重要影响.     

Ni原子双飞秒脉冲激光诱导击穿光谱的信号增强研究

在大气环境下采用波长为800nm,脉宽为30fs的飞秒激光研究了Ni的双脉冲激光诱导击穿光谱,与单飞秒脉冲激光诱导击穿光谱相比,双飞秒脉冲在最优的双脉冲相对延时下,其信号强度增强接近10倍,实验研究了双脉冲相对延时在0-1300ps范围内不同延时对激光诱导击穿光谱信号强度增强因子的影响。整个相对延时区域可以分为三个阶段：在0-50ps区域内信号增强因子是一个持续增大的过程,在50ps左右,达到一个最大值;在50-300ps区域内,信号增强因子呈现出一个先下降后上升的过程;在300-1300ps,信号增强因子基本保持不变。     

Ni原子双飞秒脉冲激光诱导击穿光谱的信号增强研究

在大气环境下采用波长为800nm,脉宽为30fs的飞秒激光研究了Ni的双脉冲激光诱导击穿光谱,与单飞秒脉冲激光诱导击穿光谱相比,双飞秒脉冲在最优的双脉冲相对延时下,其信号强度增强接近10倍,实验研究了双脉冲相对延时在0-1300ps范围内不同延时对激光诱导击穿光谱信号强度增强因子的影响。整个相对延时区域可以分为三个阶段：在0-50ps区域内信号增强因子是一个持续增大的过程,在50ps左右,达到一个最大值;在50-300ps区域内,信号增强因子呈现出一个先下降后上升的过程;在300-1300ps,信号增强因子基本保持不变。     

钾元素单脉冲和双脉冲激光诱导击穿光谱研究

基于自行研制的新型液体射流的激光诱导击穿光谱(LIBS)实验装置,研究了实验条件(如积分延时、脉冲间隔、激光能量等)对K元素单脉冲LIBS和双脉冲LIBS等离子发射的影响.实验得知相对单脉冲激光激发,双脉冲激光激发可以显著提高等离子体发射谱线强度,增加谱线强度的衰减时间,提高LIBS数据的稳定性.通过最佳实验条件下K766.49nm谱线强度随溶液浓度的分析,得到该实验系统中,双脉冲激光激发时K元素的检测灵敏度和检测限约是单脉冲激光激发时的37倍.实验结果为双脉冲LIBS技术应用于水体金属的检测提供了一定依据.     

钾元素单脉冲和双脉冲激光诱导击穿光谱研究

基于自行研制的新型液体射流的激光诱导击穿光谱(LIBS)实验装置,研究了实验条件(如积分延时、脉冲间隔、激光能量等)对K元素单脉冲LIBS和双脉冲LIBS等离子发射的影响.实验得知相对单脉冲激光激发,双脉冲激光激发可以显著提高等离子体发射谱线强度,增加谱线强度的衰减时间,提高LIBS数据的稳定性.通过最佳实验条件下K766.49nm谱线强度随溶液浓度的分析,得到该实验系统中,双脉冲激光激发时K元素的检测灵敏度和检测限约是单脉冲激光激发时的37倍.实验结果为双脉冲LIBS技术应用于水体金属的检测提供了一定依据.     

共线DP-LIBS定量分析水中Cu含量的试验研究

为研究双脉冲激光诱导击穿光谱(DP-LIBS)对水体中铜(Cu)元素检测灵敏度的影响,采用共线双脉冲LIBS检测装置对所配置的含Cu水溶液进行激光诱导击穿光谱试验。结果显示：与运用单脉冲激光诱导击穿光谱(SP-LIBS)检测水体中Cu元素相比,运用DP-LIBS探测到的光谱明显增强,并且其检测结果受光谱仪采集的延迟时间、两脉冲之间的脉冲延迟时间、双脉冲激光能量等因素的影响显著。确定最佳的试验条件为：光谱采集延迟时间为1 380 ns,脉冲延迟时间为25 ns,双脉冲激光能量为100 mJ。分别对铜元素324.7和327.4 nm的特征谱线进行定量分析,两谱线的检测限分别是3.5和4.84 μg·mL-1,且相对标准偏差都在10%以内。用500 μg·mL-1样品对特征谱线为324.7 nm所建立的定标曲线进行验证,反演得出该样品的浓度为446 μg·mL-1,相对误差为10.8%。研究表明DP-LIBS能够提高Cu元素的检测灵敏度,同时具有较高的稳定性。     

激光诱导击穿空气等离子体时间分辨特性的光谱研究

空气等离子体的时间行为对空气环境下激光诱导等离子体形成过程的研究有重要意义.本文将纳秒Nd:YAG脉冲激光(1064 nm)聚焦于一个大气压的空气中,诱导其产生等离子体.利用具有纳秒时间分辨功能的PI-MAX-II型ICCD,采用时间分辨光谱方法,研究了大气环境下激光诱导等离子体的时间行为.大气环境下的激光诱导等离子体光谱广泛分布于300—900 nm范围内,并且是由带状光谱和线状光谱叠加而成的.根据美国国家标准与技术研究院原子发射谱线数据库,对等离子体光谱中的氧、氮、氢等元素的特征谱线进行了识别和归属.给出了激光诱导击穿大气等离子体光谱随时间演化的直观图像,根据空气等离子体发射谱线计算了等离子体电子温度和等离子体电子密度.这些结果对于提高在大气环境下进行的在线测量结果的准确性和精确性具有重要的科学意义.     

Double pulse UV laser induced breakdown spectroscopy of stainless steel

Results of experimental investigations of 304 austenitic stainless steel (ASS) ultraviolet spectral range by single and double pulse laser induced breakdown spectroscopy (LIBS) at atmospheric pressure are reported. Various parameters, such as laser energy, placement of the laser beam focus with respect to the surface of illumi-nation, and collinear double laser pulse delay were used as variables. This study contributes to a better under-standing of the LIBS plasma dynamics by observing the temporal evolution of various emission lines. Temperature measurements were made by the Boltzmann diagram method using singly ionized Fe lines, and electron densities were found from Stark broadening. The temporal behaviors of these parameters were also estimated. It was found that the electron temperature for double pulses is higher than that for single pulse of the same total energy. For double pulse LIBS, the iron line emission intensities are enhanced and the analytical performance is improved. For instance, the intensity of iron line Fe I 275.01 nm was a factor of about 300 times higher if a double pulse of 2 × 20 mJ was used instead of a single pulse of 40 mJ when focusing the beam 4.7 mm behind the target surface. Published in Zhurnal Prikladnoi Spektroskopii, Vol. 79, No. 5, pp. 654–660, 2006.     

Double-pulse laser-induced breakdown spectroscopy for trace element analysis in sintered iron oxide ceramics

Double-pulse laser-induced breakdown spectroscopy (LIBS) is an emerging technique for accurate compositional analysis of many different materials. We present a systematic study of collinear double-pulse LIBS for analysis of the trace and side elements boron, manganese, copper, aluminum, titanium, silicon, chromium, nickel, potassium, and calcium in sintered iron oxide targets. The samples were ablated in air by single-pulse and double-pulse Nd:YAG laser radiation (6 ns pulse duration, laser wavelength of 532 nm) and spectra were recorded with an Echelle spectrometer equipped with an ICCD camera. We investigated the evolution of atomic and ionic line emission intensities for different interpulse delay times between the laser pulses (from 100 ns to 50 μs) and gate delays after the second laser pulse. We also varied the energy partition between the first and second laser pulse and the size of the irradiated spot at the sample surface. For the trace and side elements, we observed double-pulse LIBS signals that were enhanced as compared to single-pulse measurements depending on the interpulse delay time, the energy partition between the pulses, and the spot size. For the elements boron, copper, aluminum, titanium, chromium, potassium, and calcium limits of detection below 10 ppm were achieved.     

Double-pulse neodymium YAG/Carbon dioxide laser-induced breakdown spectroscopy for excitation of bulk and trace analytes

The mechanisms involved in signal enhancement and persistence of the plasma in double-pulse laser-induced breakdown spectroscopy are investigated, and their implications to improving figures of merit for bulk and trace analytes in sample are discussed. For double-pulse laser-induced breakdown spectroscopy, 1064 nm neodymium YAG laser is used for ablation and 10.6 µm transversely excited atmospheric carbon dioxide laser in near-collinear geometry is used for reheating. Significant improvement in signal detection and sensitivity of both bulk and trace analytes using double-pulse laser-induced breakdown spectroscopy as compared to conventional single-pulse laser-induced breakdown spectroscopy are observed. Using double-pulse laser-induced breakdown spectroscopy in near-collinear geometry, Cu and Fe as bulk and trace analytes, respectively, in brass sample, showed 5 and 6 times improvement in persistence of the spectral emission. Temporal and time-integrated studies show that ionic lines are significantly enhanced compared to neutral lines. Plasma characterization employing spectroscopic methods showed significant enhancement in plasma temperature resulting in higher signal as well as increased plasma persistence of the species studied.     

Comparison between single- and double-pulse LIBS at different air pressures on silicon target

A comparative study between single- and double-pulse laser-induced breakdown spectroscopy (LIBS) was performed on an n-type silicon(111) target. A new mobile double-pulse instrument for LIBS analysis was used for the measurements. The experiment was carried out at different air pressures of 0.7, 470 and 1000 hPa. It has been found that, in the case of double-pulse LIBS, the emission intensities of atomic and ionic lines are strongly enhanced at higher pressures. Using Stark broadening of the atomic lines of silicon, it was found that the electron number densities for single and double pulses are approximately the same (N_e∼10¹⁷ cm^-3). Plasma excitation and ionization temperatures were determined from a Boltzmann plot. The double-pulse laser-induced plasma was studied at different interpulse delay times of 1, 2, 5, 10, 15, 25 and 50 μs. The results indicated that the interaction between the laser, plasma and target gives higher atomic and ionic intensities at shorter interpulse delay times. PACS 52.38.Mf; 79.20.Ds; 52.50.Jm     

样品温度对纳秒激光诱导土壤等离子体辐射特性的影响

利用脉宽8 ns,波长为532 nm的Nd:YAG单脉冲纳秒激光器,在一个标准大气压下入射到土壤中(样品土壤来自蚌埠学院校园),改变样品温度,获得了不同样品温度下激光诱导击穿光谱. 通过分析光谱,得到土壤中不同特征谱线的强度和信噪比. 分别利用Boltzmann斜线法和Stark展宽法计算并分析了等离子体电子温度和电子密度随样品温度的演化规律;同时讨论了提高样品温度和激光诱导土壤等离子体辐射增强的原因. 实验结果表明,随着样品温度的升高,等离子体的谱线强度、信噪比、电子温度和电子密度会逐渐增强,并且在温度为100 °C时达到最大.     

Comparative Study of Two Methods of Orthogonal Double-Pulse Laser-Induced Breakdown Spectroscopy of Aluminum

Double-pulse laser induced breakdown spectroscopy (DP-LIBS) of aluminum sample is studied experimentally in orthogonal configuration in air. In this configuration, two schemes of reheating and pre-ablation are examined and the results are compared with single pulse one. The effect of delay time between two laser pulses on emission line intensities of plasma is investigated. Some of the parameters that have been involved in different mechanism of signal enhancement such as plasma temperature, sample heating effects, atmospheric effects, and modification of the ablation dynamics are more discussed. Investigation of the effect of laser pulse energy on emission line intensities in single pulse LIBS experiment demonstrate that because of saturation effects the intensities will not increase necessarily by increasing the laser pulse energy. Moreover, the results show that the electron temperature and rate of mass removal in orthogonal configuration of DP-LIBS is higher than that of single pulse with the same total energy. It is suggested that for correct comparison between single and double pulse results, the optimum pulse energy in single pulse should be considered. Overall, our results demonstrate that under optimized conditions the signal enhancement is much more in pre-ablation configuration than re-heating configuration.     

Effect of parameters on Si plasma emission in collinear double-pulse laser-induced breakdown spectroscopy

Collinear dual-pulse laser-induced breakdown spectroscopy was carried out on Si crystal by using a pair of nanosecond Nd:YAG laser sources emitting at 1064 nm. The spectral intensities and signalto-noise ratios of selected Si atomic and ionic lines were used to evaluate the optical emission. The optical emission intensity was recorded while varying the interpulse delay time and energy ratio of the two pulsed lasers. The effects of the data acquisition delay time on the line intensity and signal-to-noise ratio have been investigated as well. Based on the results, the optimal interpulse delay time, energy ratio of the two pulsed lasers, and data acquisition delay time for achieving the maximum atomic and ionic line intensities were found for generation of Si plasma with the collinear dual-pulse laser approach. The dominant mechanism for the observed line intensity variation was also discussed. In addition, the plasma temperature and electron number density at different gate delay times and different interpulse delay times were derived. A significant influence of plasma shielding on the electron temperature and electron number density at shorter interpulse delay times was observed.