Pub Date : 2025-12-02DOI: 10.1016/j.sab.2025.107419
Xing Han , Zhenxiao Li , Haibin Tang
The spectroscopic measurement method for determination of tungsten density is presented by plasma diagnostics and theoretical modeling of spectra. The collision-radiation model applicable to small amounts of tungsten in a high-density plasma is constructed to calculate the densities of neutral tungsten, singly ionized tungsten, and doubly ionized tungsten. The processes taken into account are radiative decay, electron impact excitation, electron impact deexcitation, electron impact ionization, and three-body recombination processes. The densities of different ionization states of tungsten for an applied-field magnetoplasmadynamic thruster cathode at different working currents and magnetic field intensities are diagnosed for verifying the method’s applicability. The experimental results and metallographic analysis of the material show that the lattice structure of the tungsten cathode surface has recrystallized after long-term plasma interaction, resulting in enlarged grain sizes and consequently enhanced erosion resistance.
{"title":"Tungsten collision-radiation model development and density measurement in argon plasma arc","authors":"Xing Han , Zhenxiao Li , Haibin Tang","doi":"10.1016/j.sab.2025.107419","DOIUrl":"10.1016/j.sab.2025.107419","url":null,"abstract":"<div><div>The spectroscopic measurement method for determination of tungsten density is presented by plasma diagnostics and theoretical modeling of spectra. The collision-radiation model applicable to small amounts of tungsten in a high-density plasma is constructed to calculate the densities of neutral tungsten, singly ionized tungsten, and doubly ionized tungsten. The processes taken into account are radiative decay, electron impact excitation, electron impact deexcitation, electron impact ionization, and three-body recombination processes. The densities of different ionization states of tungsten for an applied-field magnetoplasmadynamic thruster cathode at different working currents and magnetic field intensities are diagnosed for verifying the method’s applicability. The experimental results and metallographic analysis of the material show that the lattice structure of the tungsten cathode surface has recrystallized after long-term plasma interaction, resulting in enlarged grain sizes and consequently enhanced erosion resistance.</div></div>","PeriodicalId":21890,"journal":{"name":"Spectrochimica Acta Part B: Atomic Spectroscopy","volume":"237 ","pages":"Article 107419"},"PeriodicalIF":3.8,"publicationDate":"2025-12-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145737849","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-12-02DOI: 10.1016/j.sab.2025.107418
Peng Wang , Tao He , Jianyu Wang , Jiufen Liu , Feirong Meng , Qianni Men , Liming Gan , Xiaowen Jin , Boxin Feng
Activated carbon enrichment combined with flame atomic absorption spectrometry (FAAS) offers a robust approach for gold analysis in geological samples, featuring a wide determination range (e.g., 0.32–92 g t−1 in this study), good reproducibility, and high accuracy. However, its performance is influenced by multiple factors—activated carbon consumption, ash content, adsorption column layers, and washing temperature—requiring systematic optimization. This study addresses this challenge by applying an integrated model that combines the EW theory and technique for order preference by similarity to ideal solution (TOPSIS). Single-factor experiments were first conducted to determine the operational ranges for these four key parameters. A mixed orthogonal design was then implemented, using the absolute relative error (RE) at three gold concentrations (51.8, 18.3, 1.1 μg g−1) as the evaluation index. The EW method objectively assigned weights (0.3120, 0.3219, 0.3661) to these levels, and TOPSIS calculated relative closeness coefficients to rank all experiments. Range analysis identified the optimal parameter combination. Validation under optimized conditions using certified reference materials (GBW(E)070012a, GBW07808b, GBW07809a, GBW07810) confirmed high reliability, with RE and RSD values of 0.11 %–4.69 % and 0.43 %–8.35 %, respectively, complying with industry standard DZ/T 0130.3–2006. The principal novelty of this work lies in the first objective, data-driven application of the integrated EW-TOPSIS model to multi-parameter optimization in FAAS-based geochemical analysis, establishing a transferable paradigm that enhances methodological robustness and operational efficiency in analytical laboratories.
活性炭富集结合火焰原子吸收光谱法（FAAS）为地质样品中的金分析提供了一种可靠的方法，具有测定范围宽（例如，本研究的测定范围为0.32-92 g t - 1），重复性好，准确性高的特点。但其性能受活性炭用量、灰分、吸附柱层数、洗涤温度等因素的影响，需要系统优化。本研究通过应用集成模型解决了这一挑战，该模型结合了电子战理论和理想解相似性排序偏好技术（TOPSIS）。首先进行单因素实验，确定这四个关键参数的作用范围。以3种金浓度（51.8、18.3、1.1 μg−1）下的绝对相对误差（RE）为评价指标，进行混合正交设计。EW方法客观地为这些水平分配权重（0.3120,0.3219,0.3661），TOPSIS计算相对接近系数对所有实验进行排序。极差分析确定了最佳的参数组合。采用标准物质（GBW(E)070012a、GBW07808b、GBW07809a、GBW07810）在优化条件下进行验证，可靠性高，RE和RSD值分别为0.11% ~ 4.69%和0.43% ~ 8.35%，符合行业标准DZ/T 0130.3-2006。这项工作的主要新颖之处在于第一个客观的、数据驱动的综合EW-TOPSIS模型应用于基于faas的地球化学分析的多参数优化，建立了一个可转移的范例，提高了分析实验室的方法稳健性和操作效率。
{"title":"Application of the integrated entropy weight and Technique for Order of Preference by Similarity to Ideal Solution model in optimizing the sample pretreatment process for gold analysis in gold ore by Flame Atomic Absorption Spectrometry","authors":"Peng Wang , Tao He , Jianyu Wang , Jiufen Liu , Feirong Meng , Qianni Men , Liming Gan , Xiaowen Jin , Boxin Feng","doi":"10.1016/j.sab.2025.107418","DOIUrl":"10.1016/j.sab.2025.107418","url":null,"abstract":"<div><div>Activated carbon enrichment combined with flame atomic absorption spectrometry (FAAS) offers a robust approach for gold analysis in geological samples, featuring a wide determination range (e.g., 0.32–92 g t<sup>−1</sup> in this study), good reproducibility, and high accuracy. However, its performance is influenced by multiple factors—activated carbon consumption, ash content, adsorption column layers, and washing temperature—requiring systematic optimization. This study addresses this challenge by applying an integrated model that combines the EW theory and technique for order preference by similarity to ideal solution (TOPSIS). Single-factor experiments were first conducted to determine the operational ranges for these four key parameters. A mixed orthogonal design was then implemented, using the absolute relative error (RE) at three gold concentrations (51.8, 18.3, 1.1 μg g<sup>−1</sup>) as the evaluation index. The EW method objectively assigned weights (0.3120, 0.3219, 0.3661) to these levels, and TOPSIS calculated relative closeness coefficients to rank all experiments. Range analysis identified the optimal parameter combination. Validation under optimized conditions using certified reference materials (GBW(E)070012a, GBW07808b, GBW07809a, GBW07810) confirmed high reliability, with RE and RSD values of 0.11 %–4.69 % and 0.43 %–8.35 %, respectively, complying with industry standard DZ/T 0130.3–2006. The principal novelty of this work lies in the first objective, data-driven application of the integrated EW-TOPSIS model to multi-parameter optimization in FAAS-based geochemical analysis, establishing a transferable paradigm that enhances methodological robustness and operational efficiency in analytical laboratories.</div></div>","PeriodicalId":21890,"journal":{"name":"Spectrochimica Acta Part B: Atomic Spectroscopy","volume":"237 ","pages":"Article 107418"},"PeriodicalIF":3.8,"publicationDate":"2025-12-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145683058","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-12-01DOI: 10.1016/j.sab.2025.107417
Wei Zhao, Xianyun Ai, Wenhui Li
Energy resolution and matrix effects hinder the widespread application of energy-dispersive X-ray fluorescence spectroscopy in analyzing unknown samples. To address these limitations, this paper proposes a novel automatic and standardless elemental analysis method. This method integrates deconvolution with fundamental parameters model in a closed iterative framework: deconvolution first enhances spectral resolution to improve qualitative element identification, and the fundamental parameters model then quantifies elemental contents with qualitative results dynamically feeding back to input to the fundamental parameters model, forming a tightly coupled qualitative-quantitative loop. The approach was validated using multi-element certified reference materials and the results were compared with those obtained from the commercial software XRS-FP2. The findings confirm that the proposed method enables automated end-to-end elemental analysis without reference materials, and contributes to mitigating the bottlenecks of peak overlap and matrix effects in unknown sample analysis. It thus provides a practical analytical tool for rapid and reliable elemental analysis.
{"title":"An automated, standardless method for elemental analysis in EDXRF based on spectral deconvolution for resolution enhancement","authors":"Wei Zhao, Xianyun Ai, Wenhui Li","doi":"10.1016/j.sab.2025.107417","DOIUrl":"10.1016/j.sab.2025.107417","url":null,"abstract":"<div><div>Energy resolution and matrix effects hinder the widespread application of energy-dispersive X-ray fluorescence spectroscopy in analyzing unknown samples. To address these limitations, this paper proposes a novel automatic and standardless elemental analysis method. This method integrates deconvolution with fundamental parameters model in a closed iterative framework: deconvolution first enhances spectral resolution to improve qualitative element identification, and the fundamental parameters model then quantifies elemental contents with qualitative results dynamically feeding back to input to the fundamental parameters model, forming a tightly coupled qualitative-quantitative loop. The approach was validated using multi-element certified reference materials and the results were compared with those obtained from the commercial software XRS-FP2. The findings confirm that the proposed method enables automated end-to-end elemental analysis without reference materials, and contributes to mitigating the bottlenecks of peak overlap and matrix effects in unknown sample analysis. It thus provides a practical analytical tool for rapid and reliable elemental analysis.</div></div>","PeriodicalId":21890,"journal":{"name":"Spectrochimica Acta Part B: Atomic Spectroscopy","volume":"237 ","pages":"Article 107417"},"PeriodicalIF":3.8,"publicationDate":"2025-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145683116","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-11-29DOI: 10.1016/j.sab.2025.107402
Lu Wang , Xi-Ming Zhu , Tian-Yuan Ji , Yang Wang , Klaus Bartschat , Qiu-Yao Cao , Li-Qiu Wei
Metal plasma has been widely applied in hard coatings or metallization of vias and trenches in semiconductor device fabrication. Ion irradiation plays a vital role in the film properties. Previous methods have focused on the Ti atom and Ti+ ion number densities; however, there is a lack of a practical optical emission spectroscopy method for measuring the Ti2+ ion number density. High-charge-state ions lead to high compressive stress, especially in high-power impulse magnetron sputtering (HiPIMS) and vacuum arc plasma devices with a high ionization fraction. In this work, we present a novel charge-state resolved OES method to obtain the time-resolved Ti+ and Ti2+ ion number densities. This method is based on the excited-state cycle mechanisms of Ti+(4p) and Ti2+(4p) emitting states, as determined by kinetic investigations using a collisional-radiative model. In the excited-state cycle mechanisms, the Ti+/Ti2+ line-ratio is found to be sensitive to the ion ratio, and the Ti2+ line-ratio is sensitive to the electron density. The latter can decouple the influence of the electron density on the Ti+/Ti2+ line ratio, allowing the Ti+ and Ti2+ ion number densities to be determined by combining the above line ratios. This method is verified in a vacuum arc titanium metal plasma source.
{"title":"A charge-state resolved optical emission spectroscopy method applicable to vacuum-sputtered and ablated metal-containing plasma to determine the time-resolved monovalent and divalant titanium ion number densities","authors":"Lu Wang , Xi-Ming Zhu , Tian-Yuan Ji , Yang Wang , Klaus Bartschat , Qiu-Yao Cao , Li-Qiu Wei","doi":"10.1016/j.sab.2025.107402","DOIUrl":"10.1016/j.sab.2025.107402","url":null,"abstract":"<div><div>Metal plasma has been widely applied in hard coatings or metallization of vias and trenches in semiconductor device fabrication. Ion irradiation plays a vital role in the film properties. Previous methods have focused on the Ti atom and Ti<sup>+</sup> ion number densities; however, there is a lack of a practical optical emission spectroscopy method for measuring the Ti<sup>2+</sup> ion number density. High-charge-state ions lead to high compressive stress, especially in high-power impulse magnetron sputtering (HiPIMS) and vacuum arc plasma devices with a high ionization fraction. In this work, we present a novel charge-state resolved OES method to obtain the time-resolved Ti<sup>+</sup> and Ti<sup>2+</sup> ion number densities. This method is based on the excited-state cycle mechanisms of Ti<sup>+</sup>(4p) and Ti<sup>2+</sup>(4p) emitting states, as determined by kinetic investigations using a collisional-radiative model. In the excited-state cycle mechanisms, the Ti<sup>+</sup>/Ti<sup>2+</sup> line-ratio is found to be sensitive to the ion ratio, and the Ti<sup>2+</sup> line-ratio is sensitive to the electron density. The latter can decouple the influence of the electron density on the Ti<sup>+</sup>/Ti<sup>2+</sup> line ratio, allowing the Ti<sup>+</sup> and Ti<sup>2+</sup> ion number densities to be determined by combining the above line ratios. This method is verified in a vacuum arc titanium metal plasma source.</div></div>","PeriodicalId":21890,"journal":{"name":"Spectrochimica Acta Part B: Atomic Spectroscopy","volume":"237 ","pages":"Article 107402"},"PeriodicalIF":3.8,"publicationDate":"2025-11-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145737945","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-11-26DOI: 10.1016/j.sab.2025.107403
Yuji Ikeda, Joey Kim Soriano
A microwave-enhanced laser-induced breakdown spectrometer (MWE-LIBS) was developed to overcome signal attenuation in conventional LIBS and achieve higher emission intensity and signal-to-noise ratio (SNR) for spectrochemical applications. Tungsten (W) was chosen as the target material due to its high melting point and technological importance. Broadband spectra confirmed strong enhancement of both neutral (W I) and ionic (W II) emissions, with SNR values increased by nearly an order of magnitude compared to standard LIBS. Temporal measurements revealed that microwave coupling sustained plasma emission well beyond the 100 μs microwave pulse duration, supporting extended excitation and recombination cycles that favored ionic transitions. The intensity enhancement factor exceeded 400 under optimum conditions, while calibration with AlW alloys demonstrated detection limits as low as 0.036 wt% (W I) and 0.062 wt% (W II). These results establish MWE-LIBS as a robust technique for trace tungsten detection with potential applications in environmental monitoring, alloy quality control, and advanced materials analysis.
{"title":"Microwave-enhanced laser-induced breakdown spectroscopy for trace tungsten analysis","authors":"Yuji Ikeda, Joey Kim Soriano","doi":"10.1016/j.sab.2025.107403","DOIUrl":"10.1016/j.sab.2025.107403","url":null,"abstract":"<div><div>A microwave-enhanced laser-induced breakdown spectrometer (MWE-LIBS) was developed to overcome signal attenuation in conventional LIBS and achieve higher emission intensity and signal-to-noise ratio (SNR) for spectrochemical applications. Tungsten (W) was chosen as the target material due to its high melting point and technological importance. Broadband spectra confirmed strong enhancement of both neutral (W I) and ionic (W II) emissions, with SNR values increased by nearly an order of magnitude compared to standard LIBS. Temporal measurements revealed that microwave coupling sustained plasma emission well beyond the 100 μs microwave pulse duration, supporting extended excitation and recombination cycles that favored ionic transitions. The intensity enhancement factor exceeded 400 under optimum conditions, while calibration with Al<img>W alloys demonstrated detection limits as low as 0.036 wt% (W I) and 0.062 wt% (W II). These results establish MWE-LIBS as a robust technique for trace tungsten detection with potential applications in environmental monitoring, alloy quality control, and advanced materials analysis.</div></div>","PeriodicalId":21890,"journal":{"name":"Spectrochimica Acta Part B: Atomic Spectroscopy","volume":"237 ","pages":"Article 107403"},"PeriodicalIF":3.8,"publicationDate":"2025-11-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145683117","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-11-22DOI: 10.1016/j.sab.2025.107400
Muhammad Imran , Zhenhua Hu , Fang Ding , Harse Sattar , Guang-Nan Luo
In a fusion device, the high-energy ions and neutrals of impurities cause excessive erosion and redeposition of plasma-facing materials (PFMs) that lead to a reduction in fusion power output and strongly affect the divertor's lifespan. This study examined impurity types, concentration of chemical species, impurity distribution, and co-deposits on the plasma-facing components (PFCs). Collisional drag from plasma flow accelerates impurities to elevate the impact energies of impurity deposits. The test tiles of molybdenum (Mo), tungsten (W), and carbon (C) were exposed to fusion plasma in the Experimental Advanced Superconducting Tokamak (EAST) to investigate co-deposition and sputtering yield by high-energy particle bombardment and high heat flux. The redeposition patterns of local and global impurities on each test tile were analysed using laser-induced breakdown spectroscopy (LIBS) and scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX). The characterization of the test tiles reveals that enhanced gross erosion of the PFCs is caused by impurity entrainment. An uneven, thin layer co-deposited with W, Mo, Cu, Cr, Fe, Li, and Ti was observed on the test tiles. The observed high redeposition mitigates the migration of eroded materials and suppresses net erosion. Consequently, this phenomenon reduces core dilution and enhances the operational lifetime of plasma-facing components (PFCs).
{"title":"Evaluation of erosion and redeposition of irradiated plasma-facing materials by high-energy particles in fusion plasma","authors":"Muhammad Imran , Zhenhua Hu , Fang Ding , Harse Sattar , Guang-Nan Luo","doi":"10.1016/j.sab.2025.107400","DOIUrl":"10.1016/j.sab.2025.107400","url":null,"abstract":"<div><div>In a fusion device, the high-energy ions and neutrals of impurities cause excessive erosion and redeposition of plasma-facing materials (PFMs) that lead to a reduction in fusion power output and strongly affect the divertor's lifespan. This study examined impurity types, concentration of chemical species, impurity distribution, and co-deposits on the plasma-facing components (PFCs). Collisional drag from plasma flow accelerates impurities to elevate the impact energies of impurity deposits. The test tiles of molybdenum (Mo), tungsten (W), and carbon (C) were exposed to fusion plasma in the Experimental Advanced Superconducting Tokamak (EAST) to investigate co-deposition and sputtering yield by high-energy particle bombardment and high heat flux. The redeposition patterns of local and global impurities on each test tile were analysed using laser-induced breakdown spectroscopy (LIBS) and scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX). The characterization of the test tiles reveals that enhanced gross erosion of the PFCs is caused by impurity entrainment. An uneven, thin layer co-deposited with W, Mo, Cu, Cr, Fe, Li, and Ti was observed on the test tiles. The observed high redeposition mitigates the migration of eroded materials and suppresses net erosion. Consequently, this phenomenon reduces core dilution and enhances the operational lifetime of plasma-facing components (PFCs).</div></div>","PeriodicalId":21890,"journal":{"name":"Spectrochimica Acta Part B: Atomic Spectroscopy","volume":"235 ","pages":"Article 107400"},"PeriodicalIF":3.8,"publicationDate":"2025-11-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145614697","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-11-22DOI: 10.1016/j.sab.2025.107401
Zehua Liu , Ran Hai , Guoliang Xu , Zhenhua Hu , Rui Ding , Guizong Zuo , Xue Bai , Huace Wu , Cong Li , Ding Wu , Hongbin Ding
Boronization is a critical wall conditioning technique that improves the plasma performance of nuclear fusion devices by effectively reducing impurity levels. The team associated with the International Thermonuclear Experimental Reactor (ITER) has identified boronization as an effective means of mitigating the release of high-Z impurities. High-power long-pulse discharges conducted at the Experimental Advanced Superconducting Tokamak (EAST) have demonstrated the feasibility of ITER operations. A real-time monitoring of boron (B) layer thickness deposited on the first wall is crucial under these conditions. In this study, laser-induced breakdown spectroscopy (LIBS) has been applied to measure the thickness of ultra-thin boron films deposited on molybdenum (Mo) substrates at 5 × 10−5 mbar to simulate the EAST vacuum conditions. A series of boron films on Mo substrate samples with thicknesses ranging from 30 to 300 nm were produced by pulsed laser deposition (PLD). In ns-laser ablation, the first laser pulse penetrates the boron film and excites the underlying Mo substrate, producing stable spectral lines from boron (B II 703.19 nm) and molybdenum (Mo I 710.99 nm). A direct correlation is established between the intensity ratio of the B II 703.19 nm to Mo I 710.99 nm signals and the boron film thickness. A laser ablation model has been established and used to fit the experimental results, demonstrating consistency with the data. In addition, the relationship between the B/Mo signal intensity ratio and the relative amount of ablated material, calculated by calibration-free LIBS (CF-LIBS), has confirmed the validity of this approach. Based on experiments conducted using four different laser fluences, in-situ diagnostics of ultra–thin B film thickness in the 3.9–7.8 J/cm2 laser fluence range is recommended. The findings of this study have demonstrated the feasibility of LIBS technology for in-situ diagnostics of ultra-thin B layers as a means of monitoring the plasma-wall interaction (PWI) in fusion devices.
硼化是一种关键的壁调节技术，通过有效地降低杂质水平来改善核聚变装置的等离子体性能。与国际热核实验反应堆（ITER）相关的团队已经确定硼化是减轻高z杂质释放的有效手段。在实验先进超导托卡马克（EAST）上进行的高功率长脉冲放电证明了ITER运行的可行性。在这种条件下，实时监测沉积在第一壁的硼(B)层厚度至关重要。本研究采用激光诱导击穿光谱法（LIBS）测量了在5 × 10−5 mbar条件下沉积在钼（Mo）衬底上的超薄硼膜的厚度，以模拟EAST真空条件。采用脉冲激光沉积（PLD）技术在Mo衬底样品上制备了一系列厚度在30 ~ 300 nm之间的硼薄膜。在ns激光烧蚀中，第一个激光脉冲穿透硼膜，激发底层的Mo衬底，从硼（B II 703.19 nm）和钼（Mo I 710.99 nm）产生稳定的光谱线。硼膜厚度与B I 703.19 nm与Mo I 710.99 nm信号的强度比有直接的相关关系。建立了激光烧蚀模型，并对实验结果进行了拟合，结果与实验数据一致。此外，用免校准LIBS （CF-LIBS）计算了B/Mo信号强度比与烧蚀材料相对量的关系，证实了该方法的有效性。基于四种不同激光通量的实验，推荐在3.9 ~ 7.8 J/cm2激光通量范围内对超薄B膜厚度进行原位诊断。这项研究的结果证明了LIBS技术用于超薄B层原位诊断作为监测聚变装置中等离子体壁相互作用（PWI）的一种手段的可行性。
{"title":"Application of laser-induced breakdown spectroscopy to measure the thickness of ultra-thin boron films on molybdenum tiles","authors":"Zehua Liu , Ran Hai , Guoliang Xu , Zhenhua Hu , Rui Ding , Guizong Zuo , Xue Bai , Huace Wu , Cong Li , Ding Wu , Hongbin Ding","doi":"10.1016/j.sab.2025.107401","DOIUrl":"10.1016/j.sab.2025.107401","url":null,"abstract":"<div><div>Boronization is a critical wall conditioning technique that improves the plasma performance of nuclear fusion devices by effectively reducing impurity levels. The team associated with the International Thermonuclear Experimental Reactor (ITER) has identified boronization as an effective means of mitigating the release of high-Z impurities. High-power long-pulse discharges conducted at the Experimental Advanced Superconducting Tokamak (EAST) have demonstrated the feasibility of ITER operations. A real-time monitoring of boron (B) layer thickness deposited on the first wall is crucial under these conditions. In this study, laser-induced breakdown spectroscopy (LIBS) has been applied to measure the thickness of ultra-thin boron films deposited on molybdenum (Mo) substrates at 5 × 10<sup>−5</sup> mbar to simulate the EAST vacuum conditions. A series of boron films on Mo substrate samples with thicknesses ranging from 30 to 300 nm were produced by pulsed laser deposition (PLD). In ns-laser ablation, the first laser pulse penetrates the boron film and excites the underlying Mo substrate, producing stable spectral lines from boron (B II 703.19 nm) and molybdenum (Mo I 710.99 nm). A direct correlation is established between the intensity ratio of the B II 703.19 nm to Mo I 710.99 nm signals and the boron film thickness. A laser ablation model has been established and used to fit the experimental results, demonstrating consistency with the data. In addition, the relationship between the B/Mo signal intensity ratio and the relative amount of ablated material, calculated by calibration-free LIBS (CF-LIBS), has confirmed the validity of this approach. Based on experiments conducted using four different laser fluences, in-situ diagnostics of ultra–thin B film thickness in the 3.9–7.8 J/cm<sup>2</sup> laser fluence range is recommended. The findings of this study have demonstrated the feasibility of LIBS technology for in-situ diagnostics of ultra-thin B layers as a means of monitoring the plasma-wall interaction (PWI) in fusion devices.</div></div>","PeriodicalId":21890,"journal":{"name":"Spectrochimica Acta Part B: Atomic Spectroscopy","volume":"235 ","pages":"Article 107401"},"PeriodicalIF":3.8,"publicationDate":"2025-11-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145614695","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-11-21DOI: 10.1016/j.sab.2025.107399
Asmaa M. Abozied , Abdulkader M. Elmagrabi , Zein K. Heiba , Hikari Takahara , Kouichi Tsuji , Somchai Tancharakorn , Abdallah A. Shaltout
To prevent the deterioration of natural resources and support sustainable development, the valorization and recycling of various steel slags have become increasingly important. In the present work, six different types of steel slags were collected, characterized, and analyzed: electric arc furnace (EAF) slag, ladle refining furnace slag treated with Si and Al (LRF-Si and LRFAl), steel fume dust, mill scale flakes, and refractory materials waste. High resolution wavelength dispersive X-ray fluorescence (WDXRF) spectrometry with multi-dispersive crystals was used for precise quantitative elemental analysis. X-ray diffractometry was employed to identify and quantify the crystalline phases analysis within the collected samples. The analysis revealed that the mill scale flakes and EAF slags contain high concentrations of iron oxides, at approximately ∼95 % and ∼ 40 %, respectively, making them attractive for various applications. The high concentration of calcium oxides and calcium compounds in LRF slag (∼ 50 %) makes it suitable for various applications in the cement and concrete industry. Furthermore, the steel fume dust was found to contain a remarkably high concentration of zinc oxides (ZnO) reaching to ∼40 %. The high ZnO content makes the steel fume dust a promising candidate for many applications such as zinc extraction, fertilizers productions, and cosmetics.
{"title":"Valorization of steel slags through elemental and phase characterization using X-ray spectrometries","authors":"Asmaa M. Abozied , Abdulkader M. Elmagrabi , Zein K. Heiba , Hikari Takahara , Kouichi Tsuji , Somchai Tancharakorn , Abdallah A. Shaltout","doi":"10.1016/j.sab.2025.107399","DOIUrl":"10.1016/j.sab.2025.107399","url":null,"abstract":"<div><div>To prevent the deterioration of natural resources and support sustainable development, the valorization and recycling of various steel slags have become increasingly important. In the present work, six different types of steel slags were collected, characterized, and analyzed: electric arc furnace (EAF) slag, ladle refining furnace slag treated with Si and Al (LRF-Si and LRF<img>Al), steel fume dust, mill scale flakes, and refractory materials waste. High resolution wavelength dispersive X-ray fluorescence (WDXRF) spectrometry with multi-dispersive crystals was used for precise quantitative elemental analysis. X-ray diffractometry was employed to identify and quantify the crystalline phases analysis within the collected samples. The analysis revealed that the mill scale flakes and EAF slags contain high concentrations of iron oxides, at approximately ∼95 % and ∼ 40 %, respectively, making them attractive for various applications. The high concentration of calcium oxides and calcium compounds in LRF slag (∼ 50 %) makes it suitable for various applications in the cement and concrete industry. Furthermore, the steel fume dust was found to contain a remarkably high concentration of zinc oxides (ZnO) reaching to ∼40 %. The high ZnO content makes the steel fume dust a promising candidate for many applications such as zinc extraction, fertilizers productions, and cosmetics.</div></div>","PeriodicalId":21890,"journal":{"name":"Spectrochimica Acta Part B: Atomic Spectroscopy","volume":"237 ","pages":"Article 107399"},"PeriodicalIF":3.8,"publicationDate":"2025-11-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145617381","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-11-19DOI: 10.1016/j.sab.2025.107397
Jakub Buday , Jakub Výravský , Jan Cempírek , David Prochazka , Pavel Pořízka , Jozef Kaiser
Elemental mapping of light (Li, Be, B, F) and trace elements in large-area geological samples represents an analytical challenge. Increased interest in Li and rare-element deposits results in the need for reliable mapping of light and trace elements. One of the possible solutions is laser-induced breakdown spectroscopy (LIBS) combined with sophisticated data processing. We studied four large-area (ca. 8⨯8 cm) samples from two rare-element Be-rich granitic pegmatites with moderate contents of Li + Be (Maršíkov, Czech Republic) and high contents of Li + Be+B (Rau property, Yukon, Canada). Cross-sections from the host rock to the geochemically evolved center of the pegmatite were used for direct multi-element mapping, assisted semi-automated machine-learning-based mineral identification, and tracing of magmatic, metasomatic and hydrothermal processes. From the obtained LIBS data, elemental images of individual elements of interest were produced (incl. Li and Be), and unsupervised clustering to the spectra was applied. This led to cluster images manifesting the distribution of individual matrices (i.e., minerals). The outputs of clustering were visually and statistically compared to a phase map produced by a state-of-the-art SEM-EDS-based Automated mineralogy solution (TIMA) and the results show good agreement. The study demonstrates a very good applicability of LIBS for the detection and mapping of major (Si, Al, Fe, Mg, Mn, Ca, Na), light elements (Li, Be, B, F), and trace elements (Ge, Ga, Cu, Ti, Sr, Ba) in pegmatites, discerning their specific geochemical signatures corresponding to magmatic, metasomatic, and hydrothermal stage of their evolution. The EDS-based automated mineralogy offers a higher spatial resolution in general. Still, it cannot map light elements (H, Li, Be, B) and has between one to three orders of magnitude worse detection limit for many other elements (e.g. Ga…).
{"title":"Correlative imaging of large-scale geological samples using LIBS and SEM-EDX automated mineralogy","authors":"Jakub Buday , Jakub Výravský , Jan Cempírek , David Prochazka , Pavel Pořízka , Jozef Kaiser","doi":"10.1016/j.sab.2025.107397","DOIUrl":"10.1016/j.sab.2025.107397","url":null,"abstract":"<div><div>Elemental mapping of light (Li, Be, B, F) and trace elements in large-area geological samples represents an analytical challenge. Increased interest in Li and rare-element deposits results in the need for reliable mapping of light and trace elements. One of the possible solutions is laser-induced breakdown spectroscopy (LIBS) combined with sophisticated data processing. We studied four large-area (ca. 8⨯8 cm) samples from two rare-element Be-rich granitic pegmatites with moderate contents of Li + Be (Maršíkov, Czech Republic) and high contents of Li + Be+B (Rau property, Yukon, Canada). Cross-sections from the host rock to the geochemically evolved center of the pegmatite were used for direct multi-element mapping, assisted semi-automated machine-learning-based mineral identification, and tracing of magmatic, metasomatic and hydrothermal processes. From the obtained LIBS data, elemental images of individual elements of interest were produced (incl. Li and Be), and unsupervised clustering to the spectra was applied. This led to cluster images manifesting the distribution of individual matrices (i.e., minerals). The outputs of clustering were visually and statistically compared to a phase map produced by a state-of-the-art SEM-EDS-based Automated mineralogy solution (TIMA) and the results show good agreement. The study demonstrates a very good applicability of LIBS for the detection and mapping of major (Si, Al, Fe, Mg, Mn, Ca, Na), light elements (Li, Be, B, F), and trace elements (Ge, Ga, Cu, Ti, Sr, Ba) in pegmatites, discerning their specific geochemical signatures corresponding to magmatic, metasomatic, and hydrothermal stage of their evolution. The EDS-based automated mineralogy offers a higher spatial resolution in general. Still, it cannot map light elements (H, Li, Be, B) and has between one to three orders of magnitude worse detection limit for many other elements (e.g. Ga…).</div></div>","PeriodicalId":21890,"journal":{"name":"Spectrochimica Acta Part B: Atomic Spectroscopy","volume":"235 ","pages":"Article 107397"},"PeriodicalIF":3.8,"publicationDate":"2025-11-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145614696","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2025-11-17DOI: 10.1016/j.sab.2025.107387
Sandan Wang , Wanwan Cao , Jinpeng Yuan , Lirong Wang , Liantuan Xiao , Suotang Jia
Multi-channel fluorescence detection of alkali atoms offers a robust approach to overcome the intrinsically low transition probabilities of conventional single-wavelength spectroscopy and thus enhances the development of frequency standards. Here, we experimentally realize the multi-channel fluorescence spectroscopy of the Rb 5 – 7 monochromatic two-photon transition using a single 760 nm laser. Simultaneous fluorescence emissions at 780 nm, 741 nm, 795 nm, 728 nm, and approximately 420 nm are observed, consistent with the expected decay channels. The dependence of these fluorescence intensities on laser power, polarization, and vapor temperature is systematically investigated, revealing the evolution of atomic transitions under varying experimental conditions. Pressure broadening measurements of the Rb 5 – 7 transition yield a spectral linewidth of MHz. Compared with conventional single-wavelength detection at 420 nm, multi-channel approach significantly improves the signal-to-noise ratio and provides comprehensive insights into the atomic structure. These results establish a reliable foundation for developing optical frequency standards based on the Rb 5S – 7S transition.
{"title":"Multi-channel fluorescence spectroscopy of the Rb 5S1/2 – 7S1/2 transition via monochromatic two-photon excitation","authors":"Sandan Wang , Wanwan Cao , Jinpeng Yuan , Lirong Wang , Liantuan Xiao , Suotang Jia","doi":"10.1016/j.sab.2025.107387","DOIUrl":"10.1016/j.sab.2025.107387","url":null,"abstract":"<div><div>Multi-channel fluorescence detection of alkali atoms offers a robust approach to overcome the intrinsically low transition probabilities of conventional single-wavelength spectroscopy and thus enhances the development of frequency standards. Here, we experimentally realize the multi-channel fluorescence spectroscopy of the Rb 5<span><math><msub><mrow><mi>S</mi></mrow><mrow><mn>1</mn><mo>/</mo><mn>2</mn></mrow></msub></math></span> – 7<span><math><msub><mrow><mi>S</mi></mrow><mrow><mn>1</mn><mo>/</mo><mn>2</mn></mrow></msub></math></span> monochromatic two-photon transition using a single 760 nm laser. Simultaneous fluorescence emissions at 780 nm, 741 nm, 795 nm, 728 nm, and approximately 420 nm are observed, consistent with the expected decay channels. The dependence of these fluorescence intensities on laser power, polarization, and vapor temperature is systematically investigated, revealing the evolution of atomic transitions under varying experimental conditions. Pressure broadening measurements of the Rb 5<span><math><msub><mrow><mi>S</mi></mrow><mrow><mn>1</mn><mo>/</mo><mn>2</mn></mrow></msub></math></span> – 7<span><math><msub><mrow><mi>S</mi></mrow><mrow><mn>1</mn><mo>/</mo><mn>2</mn></mrow></msub></math></span> transition yield a spectral linewidth of <span><math><mo>∼</mo></math></span> <span><math><mrow><mn>1</mn><mo>.</mo><mn>08</mn><mrow><mo>(</mo><mn>2</mn><mo>)</mo></mrow></mrow></math></span> MHz. Compared with conventional single-wavelength detection at 420 nm, multi-channel approach significantly improves the signal-to-noise ratio and provides comprehensive insights into the atomic structure. These results establish a reliable foundation for developing optical frequency standards based on the Rb 5<em>S</em> – 7<em>S</em> transition.</div></div>","PeriodicalId":21890,"journal":{"name":"Spectrochimica Acta Part B: Atomic Spectroscopy","volume":"235 ","pages":"Article 107387"},"PeriodicalIF":3.8,"publicationDate":"2025-11-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145569212","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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