激光诱导击穿光谱分析中钛合金样品制备方法研究

Ti-47.5Al-2.5V-1.0Cr钛合金具有高温延展性好、高温强度大的特点,有用于铸造涡轮、涡流器、叶片等高温部件的潜力。在用激光诱导击穿光谱(LIBS)对合金或部件内部定量分析前,需预先将被分析钛合金样品和钛合金标准样品用相同的方法制备以去除表面氧化层、铸造反应层和污染物。鉴于该钛合金为室温脆性材料,不适于切削制备样品,宜采用磨抛方法制备样品,而磨抛制备样品时因发热粘滞会造成样品表面污染,影响LIBS分析钛合金中成分。实验用LIBS评价光谱磨样机磨制、金相磨样机磨制、手工磨制、手工抛光、辉光氩离子轰击等几种方法去除不同组织钛合金标样表面氧化层、污染物的效果。通过LIBS分析发现,样品制备过程中污染来源于制造砂纸的胶接剂,磨制线速度、磨料粒度、抛光方向影响制备效果,且样品的组织也影响污染物去除效果。用碳化硅砂纸光谱磨样机高速磨制钛合金表面碳污染层深度大,达15μm,高于水冷金相磨样机中速磨制的碳污染层深度,说明温度高促进碳在钛合金中的扩散;中低速磨制时,使用的砂纸标号越高,含碳、钙的污染物在样品表面附着增加。中速磨制时,与α相亲和力强的钙、铝等元素在α组织的钛合金扩散深度较α+β、α_2+γ组织钛合金大,钙污染深度达10μm,而碳在不同组织的钛合金表面扩散没有明显差别。手工低速磨制时,在钛合金表面上的碳、钙污染层较浅,深度为1~3μm,与磨痕深度一致。双向或沿磨削纹理抛光效果优于垂直纹理抛光效果,残留污染物深度不超过1μm,与辉光氩离子轰击效果相近。实验研究解决了钛合金样品制备易受污染的问题,LIBS分析碳等元素的校准曲线得到改善,测量精度得到提高。对于Ti-47.5Al-2.5V-1.0Cr钛合金样品分析的结果同其他方法的对照结果一致性较好。     

Determination of Aluminum in Nickel-Based Superalloys by Using Laser-Induced Breakdown Spectroscopy

Laser-induced breakdown spectroscopy （LIBS） was developed to detect aluminum in nickel-based superalloys （K417, GH4033, DZ125L, З ∏742y） using a non-intensified...     

激光诱导击穿光谱在铜精矿成分在线检测中的应用

目前铜精矿成分检测多为实验室离线取样检测,存在取样代表性差、检测时间长、检测结果滞后等问题。针对上述问题,实验利用基于激光诱导击穿光谱(LIBS)技术的激光成分分析仪对铜精矿中Cu、S、Fe和Si关键元素含量进行了在线检测,同时采用X射线荧光光谱仪(XRF)对相同样品采用离线检测进行对照。结果表明：激光成分分析仪在线检测结果与实验室X射线荧光光谱仪(XRF)离线检测结果相比,Cu、S、Fe和Si元素的平均绝对误差分别为0.50%、0.56%、0.65%和1.67%,平均相对误差分别为2.80%、2.28%、2.74%和12.89%,各元素重复性在线检测最大差值和相对标准偏差(RSD)均与以国家标准的化学湿法分析检测结果表征的样品不均匀性相吻合,在线检测具有较好的稳定性和重复性。基于LIBS技术的在线成分检测仪器可满足铜冶炼过程中铜精矿成分检测的实时性和可靠性要求,并为配料品质提升和冶炼工艺优化提供有力支撑。     

激光诱导击穿光谱检测铁矿石应用进展

激光诱导击穿光谱(LIBS)是一种原子发射光谱,具有实时、原位、微损、远距离、多元素同时分析等优势,在铁矿石检测领域受到关注。由于激光能量波动、基体效应、样品表面形貌等因素,LIBS在铁矿石定性、定量分析方面存在很多问题。化学计量学作为一种数据处理方法,能过滤噪声和提取有效信息,连接光谱与分析结果,对LIBS分析检测起到关键桥梁作用。近10年LIBS在铁矿石检测中的应用逐渐得到重视,LIBS可应用于鉴别铁矿石酸碱性,也可用于分析铁矿石原产地。针对铁矿石中全铁、钙、镁、硅、铝、钾、磷含量以及烧失量的定量分析,LIBS结合多变量回归已开展探索性工作,但工业应用仍不成熟。因此,如何推动LIBS在铁矿石检测领域的应用落地,仍然是一项重大挑战。     

基于磁场约束下激光诱导击穿光谱技术的重金属检测研究

为提高激光诱导击穿光谱(laser induced breakdown spectroscopy, LIBS)技术定量分析的精度,开展了磁场约束下LIBS技术对土壤中重金属元素检测的研究,并采用多谱线强度归一化内标法进行数据处理。通过比较磁场强度分别为0 T、0.3 T、0.8 T、1.25 T时的光谱特性,得到光谱强度和信噪比(signal-to-noise ratio,SNR)随磁场强度增大而增大,在1.25 T磁场强度时,样品元素Cd和Cu的光谱强度和SNR要比无磁场作用分别增强了34.77%、56.33%和40.83%、74.12%,构建了磁场强度为1.25 T时的Cd和Cu元素定量分析模型。结果显示,相对于传统内标法,采用多谱线强度归一化内标法的元素检测限分别从52.78 mg/kg和49.18 mg/kg降低到23.87 mg/kg和18.06 mg/kg;相关系数分别从0.961 3和0.942 7提高到0.996 9和0.999 3。本实验研究改善了LIBS的光谱特性,提高了定量分析的精度,采用多谱线强度归一化内标法降低了重金属的检出限和测量误差。     

激光诱导击穿光谱设备在线冰铜成分检测应用进展

利用自主研发的基于激光诱导击穿光谱(LIBS)技术的激光成分分析仪对铜冶炼现场冰铜固体和熔体成分进行了在线检测,并与取样制样后实验室的X射线荧光光谱(XRF)检测结果进行了对比.分析数据为研发设备现场投用后具备对比数据的1 294炉次,包括878炉次固体冰铜和416炉次熔体冰铜.LIBS设备在线检测与取样制样后固体XR...     

利用激光击穿光谱检测烟气中的重金属成分

搭建了一套激光击穿光谱(LIBS)实验系统, 采用Nd∶YAG脉冲激光器作为光源击穿烟气形成等离子体, 其发射光谱由中阶梯光栅光谱仪分光, 并由增强型电荷耦合器件（ICCD）进行光电探测。以煤燃烧产生的烟气和烟花爆竹燃烧产生的烟气等为对象, 获得了烟气多种重金属元素的激光击穿光谱。光谱图表明, 该技术能够同时检测烟气中的多种金属成分。以Pb元素为对象, 配置含Pb不同浓度的固体样品进行了定标实验, 结果表明, Pb谱线强度与其元素浓度成线性关系。     

Image-based plasma morphology determination and LIBS spectra correction in combustion environments

Spectra correction is essential for the quantification of laser-induced breakdown spectroscopy (LIBS) due to the uncertainties in plasma morphology. In this work, we determined the plasma morphology using a charge-coupled device camera and introduced the spectral correction method based on plasma images to a combustion environment. The plasma length, width, volume, and location were extracted from the plasma images. Using a back-scattering setup, the contribution of plasma location fluctuation to the total spectral fluctuation was mitigated. The integral intensity of the plasma image was used as a proxy of the total number density to correct the spectra. Linear relationships were established between the integral intensities of the plasma images and the spectral intensities, under different laser energy levels and gas temperatures. The image-based correction method could significantly reduce the fluctuation of raw spectral intensities when the laser energy was below 240 mJ. Compared with the correction method based on total spectral areas, the proposed method offered significant improvements in the low energy region, which promises to reduce the signal fluctuations in combustion environments while preserving the spatial resolution and mitigating the flow disturbance.     

Feasibility of laser-induced breakdown spectroscopy (LIBS) as an at-line validation tool for calcium determination in infant formula

In this study, a 150 mJ laser-induced breakdown spectroscopy (LIBS) system was assessed to determine calcium content in infant formula (IF) samples. LIBS is a promising emission spectroscopic technique for elemental analysis, which offers advantages over conventional methods such as real-time analyses, little to no sample preparation and ease of use. The aim of this work was to evaluate the feasibility of LIBS as an at-line tool for IF manufacturing. To this end, IF mixtures with varying content of calcium were prepared over a range (approx. 1.5–7 mg/g of calcium) selected to be in conformity with the guidelines provided by the Codex Alimentarius Commission. Atomic Absorption Spectroscopy (AAS) was used as the reference method for mineral content determination in IF. Partial least squares regression (PLSR) was applied to the LIBS spectral data to develop a calibration model for calcium content quantification. A validation approach was then carried out to investigate the robustness of the model, which showed a good fit with values of R²_cv of 0.90 for cross-validation and a R²_p 0.85 for external validation. Low values for root mean square errors of cross-validation (RMSECV) and prediction (RMSEP) of 0.62 mg/g and 0.68 mg/g were obtained. Furthermore, this study also illustrated the possibility of LIBS to provide mineral prediction maps as a useful tool for testing sample homogeneity.     

纳米金颗粒提高LIBS定量分析精度研究

在纳米金颗粒作用下对激光诱导击穿光谱技术(laser induced breakdown spectroscopy,LIBS)定量分析精度与检出限进行了一定的研究。LIBS在纳米金颗粒作用下,以Ni II 221.648 nm、Fe II 258.588 nm分别为分析谱线和内标元素谱线,利用标准样品不锈钢303,304,316,321,347进行定标拟合,用不锈钢310样品谱线进行精度及检出限分析。结果显示,纳米金颗粒可有效增强光谱强度,使定标曲线拟合系数得到明显提高,而且不锈钢310样品检测浓度更为准确,Ni元素的探测下限降低了1.98倍。