Diagnostics of First Wall Materials in Device by Polarization-Resolved a Magnetically Confined Fusion Laser-Induced Breakdown Spectroscopy

Laser-induced breakdown spectroscopy （LIBS） is a powerful analytical tool for real- time diagnostics and detection of multiple elements deposited at the first wall of magnetically confined plasma ft~sion devices. Recently, we have tested LIBS in our laboratory for application to in situ real-time diagnostics in the fusion device EAST. In this study, we applied polarization- resolved LIBS （PR-LIBS） to reduce the background continuum and enhance the resolution and sensitivity of LIBS. We used aluminium （A1） （as a substitute for Be） and the first wall materials tungsten （W） and molybdenum （Mo） to investigate polarized continuum emission and signal-to- background ratio （SBR）. A Nd：YAG laser with first, second and third harmonics was used to produce plasma. The effects of the laser polarization plane, environmental pressure and polarizer detection angle were investigated. The spectra obtained without using a polarizer （i.e. LIBS） were compared with those obtained with a polarizer （PR-LIBS）. Distribution of emission spectral intensity was observed to follow Malus＇ law with respect to variation in the angle of detection of the polarizer. The spectra obtained by PR-LIBS had a higher SBR and greater stability than those obtained by LIBS, thereby enhancing the reliability of LIBS for quantitative analyses. A comparison of A1, Mo and W showed that W exhibited a higher continuum with stronger polarization than the low-Z elements.     

Determination of Iron in Water Solution by Time-Resolved Femtosecond Laser-Induced Breakdown Spectroscopy

The influence of the energy of femtosecond laser pulses on the intensity of Fe I (371.99 nm) emission line and the continuous spectrum of the plasma generated on the surface of Fe3+ water solution by a Ti: sapphire laser radiation with pulse duration <45 fs and energies up to 7 mJ is determined. A calibration curve was obtained for Fe3+ concentration range from 0.5 g/L to the limit of detection in water solution, and its saturation was detected for concentrations above 0.25 g/L, which is ascribed to self-absorption. The 3σ-limit of detection obtained for Fe in water solution is 2.6 mg/L in the case of 7 mJ laser pulse energy. It is found that an increase of laser pulse energy insignificantly affects on LOD in the time-resolved LIBS and leads to a slight improvement of the limit of detection.     

Spatial Resolution Measurements of C,Si and Mo Using LIBS for Diagnostics of Plasma Facing Materials in a Fusion Device

Recently,a laser-induced breakdown spectroscopic(LIBS) system has been developed for in situ measurements of the chemical compositions of plasma facing materials(PFMs)in the Experimental Advanced Superconducting Tokamak(EAST).In this study,a LIBS system,which was used in a similar optical configuration to the in situ LIBS system in EAST,has been developed to investigate the spatial distribution of PFM elements at 1CP4 Pa.The aim of this study was to understand the nature of the spatial distribution of atoms or ions of different elements in the plasma plume and optimize the signal to background ratio for the in situ LIBS diagnosis in EAST.The spatial profiles of the LIBS signals of C,Si,Mo and the continuous background were measured.Moreover,the influence of laser spot size and laser energy density on the LIBS signals of C,Si,Mo and H was also investigated.The results show that the distribution of the C,Si and Mo peaks' intensities first increased and then decreased from the center to the edge of the plasma plume.There was a maximum value at R≈1.5 mm from the center of the plasma plume.This work aims to improve the understanding of ablating plasma dynamics in very low pressure environments and give guidance to optimize the LIBS system in the EAST device.     

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...     

Rapid Detection of Oil Pollution in Soil by Using Laser-Induced Breakdown Spectroscopy

Detection of oil pollution in soil has been carried out using laser-induced breakdown spectroscopy(LIBS). A pulsed neodymium-doped yttrium aluminum garnet(Nd:YAG) laser(1,064 nm, 8 ns, 200 mJ) was focused onto pelletized soil samples. Emission spectra were obtained from oil-contaminated soil and clean soil. The contaminated soil had almost the same spectrum profile as the clean soil and contained the same major and minor elements. However, a C–H molecular band was clearly detected in the oil-contaminated soil, while no C–H band was detected in the clean soil. Linear calibration curve of the C–H molecular band was successfully made by using a soil sample containing various concentrations of oil. The limit of detection of the C–H band in the soil sample was 0.001 mL/g. Furthermore, the emission spectrum of the contaminated soil clearly displayed titanium(Ti) lines, which were not detected in the clean soil. The existence of the C–H band and Ti lines in oil-contaminated soil can be used to clearly distinguish contaminated soil from clean soil. For comparison, the emission spectra of contaminated and clean soil were also obtained using scanning electron microscope-energy dispersive X-ray(SEM/EDX) spectroscopy,showing that the spectra obtained using LIBS are much better than using SEM/EDX, as indicated by the signal to noise ratio(S/N ratio).     

Quantitative Analysis of Mg in Pipeline Dirt Based on Laser-Induced Breakdown Spectroscopy

In order to maintain the pipeline better and remove the dirt more effectively,it was necessary to analyze the contents of elements in dirt.Mg in soil outside of the pipe and the dirt inside of the pipe was quantitatively analyzed and compared by using the laser-induced breakdown spectroscopy(LIBS).Firstly,Mg was quantitatively analyzed on the basis of Mg Ⅰ 285.213 nm by calibration curve for integrated intensity and peak intensity of the spectrum before and after subtracting noise,respectively.Then calibration curves on the basis of Mg Ⅱ 279.553 nm and MgⅡ 280.270 nm were analyzed.The results indicated that it is better to use integrated intensity after subtracting noise of the spectrum line with high relative intensity to make the calibration curve.     

Deposition Mitigation of the First Mirrors Exposed in EAST with Metal and Carbon Mixed Wall Materials

In order to investigate the effect of aperture geometry on deposition mitigation, stainless steel （SS） first mirrors （FMs） were fixed on the holders of protective aperture geometry with different depth-diameter ratios （DDRs） and exposed in the deposition dominated environment of EAST. A baffle was used during the wall conditioning. The surface properties and reflectivity of the FMs were characterized before and after exposure. It is shown that using aperture geometry and a baffle can effectively mitigate the impurities deposition. The degradation of the surface and specular reflectivity of the FMs is reduced with the increase of DDRs in the range of 0 to 2. The main contaminated elements in a low-Z and high-Z mixed wall materials environment were still carbon and oxygen.     

Characterization of the Delamination Defects in Marine Steel Using Laser-Induced Breakdown Spectroscopy

In this paper,two types of comparison analyses,bulk analysis and defect analysis,were carried out for marine steel.The results of laser-induced breakdown spectroscopy(LIBS)were compared with those of spark optical emission spectrometry(Spark-OES) and scanning electron microscopy/energy dispersion spectroscopy(SEM/EDS) in the bulk and defect analyses.The comparison of the bulk analyses shows that the chemical contents of C,Si,Mn,P,S and Cr obtained from LIBS agree well with those determined using Spark-OES.The LIBS is slightly less precise than Spark-OES.Defects were characterized in the two-dimensional distribution analysis mode for Al,Mg,Ca,Si and other elements.Both the LIBS and SEM/EDS results show the enrichment of Al,Mg,Ca and Si at the defect position and the two methods agree well with each other.SEM/EDS cannot provide information about the difference in the chemical constituents when the differences between the defect position and the normal position are not significant.However,LIBS can provide this information,meaning that the sensitivity of LIBS is higher than that of SEM/EDS.LIBS can be used to rapidly characterize marine steel defects and provide guidance for improving metallurgical processes.     

Quantitative Analysis of Carbon Content in Bituminous Coal by Laser-Induced Breakdown Spectroscopy Using UV Laser Radiation

The carbon content of bituminous coal samples was analyzed by laser-induced break?down spectroscopy. The 266 nm laser radiation was utilized for laser ablation and plasma gener?ation in air. The partial least square method and the dominant factor based PLS method were used to improve the measurement accuracy of the carbon content of coal. The results showed that the PLS model could achieve good measurement accuracy, and the dominant factor based PLS model could further improve the measurement accuracy. The coefficient of determination and the root-mean-square error of prediction of the PLS model were 0.97 and 2.19%, respectively; and those values for the dominant factor based PLS model were 0.99 and 1.51%, respectively. The results demonstrated that the 266 nm wavelength could accurately measure the carbon content of bituminous coal.     

Development of a Laboratory Cement Quality Analysis Apparatus Based on Laser-Induced Breakdown Spectroscopy

Determination of the chemical composition of cement and ratio values of clinker plays an important role in cement plants as part of the optimal process control and product quality evaluation. In the present paper, a laboratory laser-induced breakdown spectroscopy (LIBS) apparatus mainly comprising a sealed optical module and an analysis chamber has been designed for possible application in cement plants for on-site quality analysis of cement. Emphasis is placed on the structure and operation of the LIBS apparatus, the sealed optical path, the temperature controlled spectrometer, the sample holder, the proper calibration model established for minimizing the matrix effects, and a correction method proposed for overcoming the ‘drift’ obstacle. Good agreement has been found between the laboratory measurement results from the LIBS method and those from the traditional method. The absolute measurement errors presented here for oxides analysis are within 0.5%, while those of ratio values are in the range of 0.02 to 0.05. According to the obtained results, this laboratory LIBS apparatus is capable of performing reliable and accurate, composition and proximate analysis of cement and is suitable for application in cement plants.     

Simultaneous Determination of Trace Lead and Chromium in Water Using Laser-Induced Breakdown Spectroscopy and Paper Substrate

Toxic metals such as lead and chromium in aqueous solutions have been analyzed simultaneously by laser-induced breakdown spectroscopy(LIBS), in which the ordinary printing paper is used as a liquid absorber which was immerged into Pb(NO3)2and Cr(NO3)3aqueous solution to enrich the heavy metals. This method overcomes the drawbacks of splashing and low sensitivity in ordinary LIBS analysis of water, in which a laser beam is directly focused on a liquid surface. A good signal intensity and reproducibility has been demonstrated. The Pb 405.78 nm and Cr 427.48 nm spectral lines are used as the analytical lines. The variation of line intensity with immersion time was investigated. The calibration curve for quantitative measurement of Pb and Cr in water was established, and the detection limits are 0.033 mg/L and 0.026 mg/L respectively,which is about 2-3 orders of magnitude better than that in the ordinary LIBS analysis of heavy metal in solution.     

Effect of Melting Iron-Based Alloy Temperature on Carbon Content Observed in Laser-Induced Breakdown Spectroscopy

Our recent work has determined the carbon content in a melting ferroalloy by laser-induced breakdown spectroscopy (LIBS). The emission spectrum of carbon that we obtained in the laboratory is suitable for carbon content determination in a melting ferroalloy but we cannot get the expected results when this method is applied in industrial conditions: there is always an unacceptable error of around 4% between the actual value and the measured value. By comparing the measurement condition in the industrial condition with that in the laboratory, the results show that the temperature of the molten ferroalloy samples to be measured is constant under laboratory conditions while it decreases gradually under industrial conditions. However, temperature has a considerable impact on the measurement of carbon content, and this is the reason why there is always an error between the actual value and the measured value. In this paper we compare the errors of carbon content determination at different temperatures to find the optimum reference temperature range which can fit the requirements better in industrial conditions and, hence, make the measurement more accurate. The results of the comparative analyses show that the measured value of the carbon content in molten state (1620 K) is consistent with the nominal value of the solid standard sample (error within 0.7%). In fact, it is the most accurate measurement in the solid state. Based on this, we can effectively improve the accuracy of measurements in laboratory and can provide a reference standard of temperature for the measurement in industrial conditions.     

A Study of the Laser-Induced Breakdown Spectroscopy of Carbon in the Ultraviolet Wavelength Range Under Vacuum Conditions

The influence of a vacuum on the laser-induced breakdown spectroscopy(LIBS) of carbon in the ultraviolet wavelength range is studied.Experiments are performed with graphite using a LIBS system,which consists of a 1064 nm Nd:YAG laser,a vacuum pump,a spectrometer and a vacuum chamber.The vacuum varies from 10 Pa to 1 atm.Atomic lines as well as singly and doubly charged ions are confirmed under the vacuums.A temporal evolution analysis of intensity is performed for the atomic lines of C Ⅰ 193.09 nm and C Ⅰ 247.86 nm under different vacuum conditions.Both time-integrated and time-resolved intensity evolutions under vacuums are achieved.The lifetimes of the two atomic lines have similar trends,which supports the point of view of a 'soft spot'.Variations of plasma temperature and electron density under different vacuums are measured.This study is helpful for research on carbon detection using LIBS under vacuum conditions.     

聚变堆第一壁用纳米结构ODS钢的发展与前瞻

第一壁结构材料必须满足聚变堆极其严酷的工作环境要求,这是制约聚变堆发展的技术瓶颈之一。近年来发展起来的纳米结构氧化物弥散强化钢的特征性微观结构赋予了该材料优异的抗辐照性能,被视为第一壁结构材料的发展方向。本文简述了国内外第一壁材料的研究与发展概况。     

Analysis of Pulverized Coal by Laser-Induced Breakdown Spectroscopy

Laser-induced breakdown spectroscopy （LIBS） has been used to detect atomic species in various enviromnents. The quantitative analysis （C, H, O, N and S） of representative coal samples are being carried out with LIBS, and the effects of particle size are analyzed. A powerful pulse Nd：YAG laser is focused on the coal sample at atmosphere pressure, and the emission spectra from laser-induced plasmas are measured by time-resolved spectroscopy, and the intensity of analyzed spectral lines is obtained through observing the laser plasma with a delay time of 0.4 #s. The experimental results show that the slope of calibration curve is nearly 1 when the concentration of the analyzed element is relatively low, and the slope of curve is nearly 0.5 when the concentration of C is higher than other elements. In addition, using the calibration-free model without self-absorption effect, the results show that the decreasing of particle size leads to an increase of the plasma temperature.     

聚变堆螺旋流道液态第一壁流动稳定性分析

聚变堆包层第一壁材料所面临高能粒子辐照、电磁辐射、高热负荷、复杂的机械负荷和相应的物理化学腐蚀制约其服役性能和使用寿命,是聚变能发展的瓶颈问题。液态第一壁由于液态工质自身的特点可以承受更高的热负载、中子壁负载以及更高的出口温度,且由于液态工质的不断更新不存在中子辐照损伤问题,在未来聚变堆应用中很具有吸引力。但由于液态金属在聚变堆强磁场作用下流动形成磁流体(Magnetohydrodynamic MHD)效应,维持液态第一壁在复杂的几何结构和苛刻的工作条件的稳定流动性是现有液态壁研究的难点问题。本文针对自由表面液态金属流动时产生的MHD特性,提出了螺旋流道液态壁流动方案,通过在真空室背壁上设置沿磁场方向的螺旋型流道,使流道内液态金属沿磁场运动,进而减少切割磁场产生的MHD效应。并参考典型聚变堆FDS-Ⅱ,建立了外包层三维模型与真实磁场位型,对方案进行MHD分析与优化,分析结果表明该方案可以在真空室表面形成完整、稳定的液态金属包裹,验证了该方案在磁场作用下液态第一壁流动稳定性与初步可行性。     

Radiative Heat Deposition Analysis of Fusion Reactor First Wall by Monte Carlo Transport Code

Heat flux distribution on the first wall of a fusion reactor due to the thermal radiation from high temperature protection wall placed in front of the first wall was analyzed. With necessary modifications, a three-dimensional Monte Carlo transport code developed for neuronics calculation was successfully applied in the analysis. That is, reasonable results with sufficiently small statistical error were obtained with reasonable computational time. The heat flux distribution was found to be insensitive to the reflection characteristic of the radiation at the first wall i. e. diffusive or specular.     

The Enhanced Effect of Optical Emission from Laser Induced Breakdown Spectroscopy of an Al-Li Alloy in the Presence of Magnetic Field Confinement

In this paper,the influence of magnetic field strength on laser-induced breakdown spectroscopy(LIBS) has been investigated for various pressures.The plasma plume was produced by employing Q-switch Nd:YAG laser ablation of an Al-Li alloy operating at a 1064 nm wavelength.The results indicated that the LIBS intensity of the Al and Li emission lines is boosted with an increase of magnetic strength.Typically,the intensity of the Al Ⅰ and Li Ⅰ spectral emissions can be magnified by 1.5-3 times in a steady magnetic field of 1.1 T compared with the field-free case.Also,in this investigation we recorded time-resolved images of the laser-produced plume by employing a fast ICCD camera.The results show that the luminance of the plasma is enhanced and the time of persistence is increased significantly,and the plasma plume splits into two lobes in the presence of a magnetic field.The probable reason for the enhancement is the magnetic confinement effect which increases the number density of excited atoms and the population of species in a high energy state.In addition,the electron temperature and density are also augmented by the magnetic field compared to the field-free case.     

A Hydrogel's Formation Device for Quick Analysis of Liquid Samples Using Laser-Induced Breakdown Spectroscopy

The laser-induced breakdown spectroscopy technique has irreplaceable advantages in the field of detection due to its multi-phase specimen detection ability.The development of the LIBS technique for liquid analysis is obstructed by its inherent drawbacks like the surface ripples and extinction of emitted intensity,which make it unpractical.In this work,an in-situ hydrogel formation sampling device was designed and used the hydrogel as the detection phase of LIBS for Cu,Cr and Al in an aqueous solution.With the measured amount of resin placed in the device,the formed hydrogel could be obtained within 20 s after putting the device into water solution.The formed hydrogel could be directly analyzed by LIBS and reflect the elemental information of the water sample.The prominent performance made this hydrogel's formation device especially suitable for quick in-situ environmental liquid analysis using LIBS.     

Signal Detection of Carbon in Iron-Based Alloy by Double-Pulse Laser-Induced Breakdown Spectroscopy

Although single-pulse lasers are often used in traditional laser-induced breakdown spectroscopy (LIBS) measurements, their measurement outcomes are generally undesirable be?cause of the low sensitivity of carbon in iron-based alloys. In this article, a double-pulse laser was applied to improve the signal intensity of carbon. Both the inter-pulse delay and the combina?tion of laser wavelengths in double-pulse laser-induced breakdown spectroscopy (DP-LIBS) were optimized in our experiment. At the optimized inter-pulse delay, the combination of a first laser of 532 nm and a second laser of 1,064 nm achieved the highest signal enhancement. The proper?ties of the target also played a role in determining the mass ablation enhancement in DP-LIBS con?guration.