Patterning single-layer materials by electrical breakdown using atomic force microscopy

The development of nanoelectronics and nanotechnologies has been boosted significantly by the emergence of 2D materials because of their atomic thickness and peculiar properties,and developing a universal,precise patterning technology for single-layer 2D materials is critical for assembling nanodevices.Demonstrated here is a nanomachining technique using electrical breakdown by an AFM tip to fabricate nanopores,nanostrips,and other nanostructures on demand.This can be achieved by voltage scanning or applying a constant voltage while moving the tip.By measuring the electrical current,the formation process on single-layer materials was shown quantitatively.The present results provide evidence of successful pattern fabrication on single-layer MoS2,boron nitride,and graphene,although further confirmation is still needed.The proposed method holds promise as a general nanomachining technology for the future.

Characteristics of laser-induced breakdown spectroscopy of liquid slag

Rapid online analysis of liquid slag is essential for optimizing the quality and energy efficiency of steel production. To investigate the key factors that affect the online measurement of refined slag using laser-induced breakdown spectroscopy(LIBS), this study examined the effects of slag composition and temperature on the intensity and stability of the LIBS spectra. The experimental temperature was controlled at three levels: 1350℃, 1400℃, and 1450℃. The results showed that slag composition and temperature significantly affected the intensity and stability of the LIBS spectra. Increasing the Fe content and temperature in the slag reduces its viscosity, resulting in an enhanced intensity and stability of the LIBS spectra. Additionally, 42 refined slag samples were quantitatively analyzed for Fe, Si, Ca, Mg, Al, and Mn at 1350℃, 1400℃, and 1450℃.The normalized full spectrum combined with partial least squares(PLS) quantification modeling was used, using the Ca Ⅱ 317.91 nm spectral line as an internal standard. The results show that using the internal standard normalization method can significantly reduce the influence of spectral fluctuations. Meanwhile, a temperature of 1450℃ has been found to yield superior results compared to both 1350℃ and 1400℃, and it is advantageous to conduct a quantitative analysis of the slag when it is in a “water-like” state with low viscosity.

Estimating the yield stress of soft materials via laser-induced breakdown spectroscopy

Taking three typical soft samples prepared respectively by loose packings of 77-,95-,and 109-μm copper grains as examples,we perform an experiment to investigate the energy-dependent laser-induced breakdown spectroscopy(LIBS)of soft materials.We discovered a reversal phenomenon in the trend of energy dependence of plasma emission intensity:increasing initially and then decreasing separated by a well-defined critical energy.The trend reversal is attributed to the laser-induced recoil pressure at the critical energy just matching the sample's yield strength.As a result,a one-to-one correspondence can be well established between the samples'yield stress and the critical energy that is easily obtainable from LIBS measurements.This allows us to propose an innovative method for estimating the yield stress of soft materials via LIBS with attractive advantages including in-situ remote detection,real-time data collection,and minimal destructive to sample.

Phase field model for electric-thermal coupled discharge breakdown of polyimide nanocomposites under high frequency electrical stress

In contrast to conventional transformers, power electronic transformers, as an integral component of new energy power system, are often subjected to high-frequency and transient electrical stresses, leading to heightened concerns regarding insulation failures. Meanwhile, the underlying mechanism behind discharge breakdown failure and nanofiller enhancement under high-frequency electrical stress remains unclear. An electric-thermal coupled discharge breakdown phase field model was constructed to study the evolution of the breakdown path in polyimide nanocomposite insulation subjected to high-frequency stress. The investigation focused on analyzing the effect of various factors, including frequency, temperature, and nanofiller shape, on the breakdown path of Polyimide(PI) composites. Additionally, it elucidated the enhancement mechanism of nano-modified composite insulation at the mesoscopic scale. The results indicated that with increasing frequency and temperature, the discharge breakdown path demonstrates accelerated development, accompanied by a gradual dominance of Joule heat energy. This enhancement is attributed to the dispersed electric field distribution and the hindering effect of the nanosheets. The research findings offer a theoretical foundation and methodological framework to inform the optimal design and performance management of new insulating materials utilized in high-frequency power equipment.

A data selection method for matrix effects and uncertainty reduction for laser-induced breakdown spectroscopy

Severe matrix effects and high signal uncertainty are two key bottlenecks for the quantitative performance and wide applications of laser-induced breakdown spectroscopy(LIBS).Based on the understanding that the superposition of both matrix effects and signal uncertainty directly affects plasma parameters and further influences spectral intensity and LIBS quantification performance,a data selection method based on plasma temperature matching(DSPTM)was proposed to reduce both matrix effects and signal uncertainty.By selecting spectra with smaller plasma temperature differences for all samples,the proposed method was able to build up the quantification model to rely more on spectra with smaller matrix effects and signal uncertainty,therefore improving final quantification performance.When applied to quantitative analysis of the zinc content in brass alloys,it was found that both accuracy and precision were improved using either a univariate model or multiple linear regression(MLR).More specifically,for the univariate model,the root-mean-square error of prediction(RMSEP),the determination coefficients(R^(2))and relative standard derivation(RSD)were improved from 3.30%,0.864 and 18.8%to 1.06%,0.986 and 13.5%,respectively;while for MLR,RMSEP,R^(2)and RSD were improved from 3.22%,0.871 and 26.2%to 1.07%,0.986 and 17.4%,respectively.These results prove that DSPTM can be used as an effective method to reduce matrix effects and improve repeatability by selecting reliable data.

Self-absorption effects of laser-induced breakdown spectroscopy under different gases and gas pressures

The self-absorption effect is one of the main factors affecting the quantitative analysis accuracy of laser-induced breakdown spectroscopy.In this paper,the self-absorption effects of laserinduced 7050 Al alloy plasma under different pressures in air,Ar,and N2have been studied.Compared with air and N2,Ar significantly enhances the spectral signal.Furthermore,the spectral self-absorption coefficient is calculated to quantify the degree of self-absorption,and the influences of gas species and gas pressure on self-absorption are analyzed.In addition,it is found that the spectral intensity fluctuates with the change of pressure of three gases.It can also be seen that the fluctuation of spectral intensity with pressure is eliminated after correcting,which indicates that the self-absorption leads to the fluctuation of spectral intensity under different pressures.The analysis shows that the evolution of optical thin spectral lines with pressure in different gases is mainly determined by the gas properties and the competition between plasma confinement and Rayleigh–Taylor instability.

Influence of the electrolyte conductivity on the critical current density and the breakdown voltage

The work investigates influence of the electrolyte conductivity on the onset of partial contact glow discharge electrolysis(CGDE)in a water electrolysis.Critical current density(CCD)and breakdown voltage were measured together with in situ observation of hydrogen bubble behavior,whose influence has not been focused on.For a fixed current during normal electrolysis,hydrogen coalescence adjacent to cathode surface was invigorated at a lower conductivity.Photographic analyses elucidated the hydrogen coalescence characteristics by quantifying size and population of detached hydrogen bubbles.The CCD increased about 104% within given range of conductivity(11.50-127.48 mS·cm^(-1))due to impaired bubble coalescence,which delays hydrogen film formation on the cathode.Meanwhile,decreasing trend of breakdown voltage was measured with increased conductivity showing maximum drop of 74%.It is concluded that onset of partial CGDE is directly affected by hydrodynamic bubble behaviors,whereas the electrolyte conductivity affects the bubble formation characteristics adjacent to cathode electrode.

Matrix effect suppressing in the element analysis of soils by laser-induced breakdown spectroscopy with acoustic correction

Laser-induced breakdown spectroscopy(LIBS)has been used for soil analysis,but its measurement accuracy is often influenced by matrix effects of different kinds of soils.In this work,a method for matrix effect suppressing was developed using laser-induced plasma acoustic signals to correct the original spectrum,thereby improving the analysis accuracy of the soil elements.A good linear relationship was investigated firstly between the original spectral intensity and the acoustic signals.The relative standard deviations(RSDs)of Mg,Ca,Sr,and Ba elements were then calculated for both the original spectrum and the spectrum with the acoustic correction,and the RSDs were significantly reduced with the acoustic correction.Finally,calibration curves of MgⅠ285.213 nm,CaⅠ422.673 nm,SrⅠ460.733 nm and BaⅡ455.403 nm were established to assess the analytical performance of the proposed acoustic correction method.The values of the determination coefficient(R~2)of the calibration curves for Mg,Ca,Sr,and Ba elements,corrected by the acoustic amplitude,are improved from 0.9845,0.9588,0.6165,and 0.6490 to 0.9876,0.9677,0.8768,and 0.8209,respectively.The values of R~2 of the calibration curves corrected by the acoustic energy are further improved to 0.9917,0.9827,0.8835,and 0.8694,respectively.These results suggest that the matrix effect of LIBS on soils can be clearly improved by using acoustic correction,and acoustic energy correction works more efficiently than acoustic amplitude correction.This work provides a simple and efficient method for correcting matrix effects in the element analysis of soils by acoustic signals.

Detection and quantification of Pb and Cr in oysters using laser-induced breakdown spectroscopy

The quantitative determination of heavy metals in aquatic products is of great importance for food security issues.Laser-induced breakdown spectroscopy(LIBS)has been used in a variety of foodstuff analysis,but is still limited by its low sensitivity when targeting trace heavy metals.In this work,we compare three sample enrichment methods,namely drying,carbonization,and ashing,for increasing detection sensitivity by LIBS analysis for Pb and Cr in oyster samples.The results demonstrate that carbonization can remove a significant amount of the contributions of organic elements C,H,N and O;meanwhile,the signals of the metallic elements such as Cu,Pb,Sr,Ca,Cr and Mg are enhanced by3–6 times after carbonization,and further enhanced by 5–9 times after ashing.Such enhancement is not only due to the more concentrated metallic elements in the sample compared to the dried ones,but also the unifying of the matter in carbonized and ashed samples from which higher plasma temperature and electron density are observed.This condition favors the detection of trace elements.According to the calibration curves with univariate and multivariate analysis,the ashing method is considered to be the best choice.The limits of detection of the ashing method are 0.52 mg kg-1 for Pb and0.08 mg kg-1 for Cr,which can detect the presence of heavy metals in the oysters exceeding the maximum limits of Pb and Cr required by the Chinese national standard.This method provides a promising application for the heavy metal contamination monitoring in the aquatic product industry.

Design optimization of high breakdown voltage vertical GaN junction barrier Schottky diode with high-K/low-K compound dielectric structure

A vertical junction barrier Schottky diode with a high-K/low-K compound dielectric structure is proposed and optimized to achieve a high breakdown voltage(BV).There is a discontinuity of the electric field at the interface of high-K and low-K layers due to the different dielectric constants of high-K and low-K dielectric layers.A new electric field peak is introduced in the n-type drift region of junction barrier Schottky diode(JBS),so the distribution of electric field in JBS becomes more uniform.At the same time,the effect of electric-power line concentration at the p-n junction interface is suppressed due to the effects of the high-K dielectric layer and an enhancement of breakdown voltage can be achieved.Numerical simulations demonstrate that GaN JBS with a specific on-resistance(R_(on,sp)) of 2.07 mΩ·cm^(2) and a BV of 4171 V which is 167% higher than the breakdown voltage of the common structure,resulting in a high figure-of-merit(FOM) of 8.6 GW/cm^(2),and a low turn-on voltage of 0.6 V.

微波脉冲大气击穿临界场强估计

针对高功率微波在大气传输中可能出现的击穿现象,研究了脉冲序列中首次击穿时的延迟脉冲数,发现其与种子电子、脉冲击穿概率以及微波场强密切相关。研究发现,微波场强可通过作用于种子电子间接影响脉冲击穿概率和延迟脉冲数,由此提出利用延迟脉冲数估计微波击穿临界场强的方法,并定义在脉冲击穿概率大于一定值时的微波临界场强作为击穿阈值。推导了脉冲击穿概率的估计公式,并对估计量的性能进行了分析,随后利用S波段微波大气击穿模拟装置开展了实验验证。实验结果表明,在一定范围内,重复频率微波脉冲击穿延迟脉冲数仅与种子电子产生率和脉宽成反比,能用于估计脉冲击穿概率,进而给出击穿临界场强。

时间分辨动态LIBS测量方法

针对激光诱导击穿光谱(LIBS)研究对时间分辨动态光谱测量方法的需求,建立了基于多通道光纤束的动态LIBS测量方法。该方法首先利用不同长度的光纤组成多通道光纤束,对瞬态LIBS信号进行差异延迟,使按照特定时间序列发射的光谱信号同步到达探测器,而后采用面阵ICCD相机对同步到达的多通道光谱信号进行高时间分辨探测。该方法单次测量即可获得LIBS辐射不同时刻的时间分辨光谱。为了验证基于多通道光纤束的动态LIBS测量方法,研制了具有19个通道的光纤束,光纤束中包含的各个单根光纤长度呈等差数列排布,长度差设置为10 m,对应测量的时间间隔约为50 ns,单次测量记录的总时间长度近900 ns。分别基于短脉冲激光光源和标准光源,开展了系统时间响应和光谱响应特性研究,获得了系统的时间响应数据和光谱响应曲线。用YAG激光器的二倍频激光(532 nm)诱导Si产生等离子体辐射光谱,在线测量了辐射光谱的时间演化历程,获得了Si等离子体辐射过程中SiⅠ390.52 nm,SiⅡ385.51 nm,SiⅡ413.12 nm谱线从0~898 ns时间范围内19个时刻的光谱信息,获得了特征光谱的演化规律,验证了该测量方法的可行性。结果表明,利用该测量方法,单次测量可以获得瞬态LIBS辐射过程中19个时刻的光谱参数,具有很高的测量效率。对于实验成本较高、运行频率低的激光诱导等离子体实验研究,采用该方法可以大大降低了测量成本,有效提升等离子体时间分辨动态光谱测量能力。

LIBS结合图像筛选方法提高钢铁中Cu、Cr、Mn元素检测稳定性研究

优质特种钢材和低端粗钢之间的性能差异主要受其构成元素种类及其成分含量的影响,因此,如何快速准确地对物质成分进行定性及定量分析对钢铁产品的质量评估至关重要。针对传统方法难以实现对钢铁合金成分的快速准确检测的难题,采用激光诱导击穿光谱(LIBS)结合等离子体图像信息的方法,通过快速地对不同元素的特征光谱强度与激发生成的等离子体图像进行采集,分析两者之间的相关性,并通过提取的图像特征信息的异常值剔除了部分无效光谱数据,进而实现了对钢铁成分的高精度分析。通过分析延迟时间和激光能量等不同实验条件对元素特征光谱强度及其对应等离子体图像的影响规律,不仅证明了等离子体图像与光谱之间存在相关性,还利用等离子体图像特征信息的局部最优值确定了最优延迟时间、激光能量分别为1000 ns与50 mJ,并根据图像特征的平均阈值来筛选无效光谱数据。结果表明,图像筛选优化数据后,各元素谱线校准模型的决定系数(R^(2))分别从原始数据的0.978、0.986、0.957、0.935提升至0.995、0.997、0.968、0.957,且其定标曲线对未知样品元素的预测浓度相对标准偏差(RSD)下降为原始数据预测浓度RSD的50%左右。由此可知采用LIBS结合图像筛选方法可以减少定量分析的误差,提高预测结果精确度。

基极触发的雪崩晶体管导通机理

为研究基极触发的雪崩晶体管导通机理,建立了雪崩晶体管(n+⁃p⁃n⁃n+掺杂结构)的准三维器件模型和实验测试电路。研究了雪崩晶体管的温度分布特征,导通结束后器件最高温度约为417 K,位于电流通道内n⁃n+边界处。当集电极电压为300 V、基极触发电压为2.4 V时,仿真和实验获得的脉冲上升时间分别为2.4 ns、2.5 ns,半高宽(FWHM)分别为6.2 ns、5.8 ns,仿真和实验结果基本一致。研究结果表明:高触发脉冲电压幅值会加速晶体管内部电场的重建过程,从而缩短延迟时间,提高晶体管响应速度;负载阻抗会影响器件导通通道尺寸,负载阻抗减小时,电流密度提升,器件通过缩窄通道来提高通道内电流密度,宏观导通电阻降低。

重复频率微波脉冲大气击穿延时与电离率

针对高功率微波在大气传输中可能出现的击穿现象,研究了脉冲序列中首次脉冲击穿延时和后续脉冲击穿延时,研究结果发现首次脉冲击穿延时在脉宽范围内大致均匀分布,后续脉冲击穿延时波动性较小。根据击穿延时数据对电离率进行了分析,指出在重复频率条件下,初始电子密度较高,电子密度分布不适用指数分布,无法用延时数据标准差对电离率进行估计。提出了一种用重复频率脉冲击穿延时数据计算电离率的方法,并将计算结果与仿真结果进行了对比,结果显示,二者有较好的对应关系。

基于激光诱导击穿光谱的混凝土氯元素分布测量方法

氯元素会对混凝土结构产生侵蚀,引起结构内部的钢筋锈蚀,导致混凝土开裂,破坏结构的完整性。化学滴定等常规的混凝土中氯元素含量测量方法存在操作复杂、检测速度慢等问题。激光诱导击穿光谱(LIBS)具有无须样品预处理、二维扫描检测和原位定点分析等优势,但其用于混凝土中的氯元素含量测量仍存在氯元素定量限难以降低、非水泥成分对氯元素二维分布测量结果的影响等问题。面向核电站混凝土构筑物中氯元素含量现场快速检测的需求,研究了氯元素含量分布的双脉冲激光诱导击穿光谱检测方法,进一步评估了核电站混凝土模拟样品渗透面中氯离子的侵蚀状况。首先,分别采用内标法、主成分回归和支持向量回归建立氯元素定标模型,基于内标法得到的氯元素检测限为0.006 02 wt%、定量限为0.018 06 wt%,并采用留一法交叉验证法来评估三种模型的预测性能。其次,为了排除非水泥基质对氯元素检测的影响,分别建立了结合主成分分析的逻辑回归分类和支持向量机分类模型对混凝土中的水泥和骨料进行精确识别。同时选取Si、 Ca、 O三种元素组合的支持向量机模型的分类效果最优,其对总体组分识别的准确率达到了98.20%,其中骨料识别准确率97.84%、水泥识别准确率为98.33%。最后,基于主成分回归定标模型针对侵蚀15和30 d的混凝土渗透面的氯含量进行二维分布测量,两种样品的平均预测Cl含量均在约2 mm处达到最大值分别为0.890 wt%和0.599 wt%,结果与电位滴定法一致。综上,基于双脉冲激光诱导击穿光谱检测方法,在30 mJ的总能量下实现了氯元素检测限达0.006 02 wt%,实现了混凝土中骨料和水泥的精确识别,获得了混凝土侵蚀渗透面的氯元素含量二维分布,为核电站混凝土构筑物氯元素含量快速检测的现场应用提供了工程化解决方案。

红外偏振辐射模型对铬和铜元素的优化识别

针对优化激光诱导击穿光谱技术识别铬和铜元素的问题,本文提出了一种结合红外偏振检测理论的方法。利用菲涅尔反射定律和基尔霍夫理论分析了红外偏振产生机理,根据能量守恒定律验证了目标红外自发热辐射的偏振特性;利用红外偏振辐射传输模型及菲涅尔反射穆勒矩阵,结合温度的麦克斯韦-玻尔兹曼分布特性,推导出了等离子体红外偏振辐射信号模型,用于识别各激发能量下的重金属元素;利用5种不同能量的脉冲激光验证了模型的精准性。结果表明:在相同的激光能量下,红外偏振辐射光谱可以收集到更多的特征信号峰;在低能量激励下,红外偏振辐射光谱的优势更为突出。红外偏振辐射模型的构建是科学有效的,可用于优化重金属元素的快速检测。

激光诱导击穿光谱技术对钕铁硼永磁材料中多元素的定量表征

“磁王”钕铁硼是现今性能最为优异的永磁体,因其优异的磁性能被广泛应用于工业互联网、新能源、 5G通讯等诸多高新科技领域。目前研究钕铁硼材料中元素成分的主要分析方法有电感耦合等离子体发射光谱(ICP-OES)和X射线荧光光谱(XRF),其中ICP-OES是湿法分析,样品前处理复杂,测试周期长,而XRF法可实现直接分析,但受制于其轻元素的检测能力很难满足对钕铁硼材料中主要轻元素B的分析需求。激光诱导击穿光谱(LIBS)技术具有分析效率高,样品前处理简单,多元素直接分析,适用于现场分析、在线分析等技术优点,使其在快速定量表征方面展现出其独有的优势。运用LIBS分析技术开展对钕铁硼材料中多元素定量表征的直接、快速分析的方法研究,首先针对钕铁硼材料中定量表征的九个元素Nd、 Co、 B、 Dy、 Tb、 Pr、 Cu、 Al、 Ga完成特征谱线的筛选,通过对系统激光器电压、激光剥蚀方式等因素在不同条件下对钕铁硼材料光谱信号稳定性的影响分析,优化并确立了分析条件,最终选用720V的激光器电压,15个预剥蚀脉冲15个剥蚀脉冲的激光剥蚀方式为钕铁硼样品的分析条件;其次,选取8个通过ICP-OES法定值的烧结钕铁硼样品,样品具有元素成分的梯度差异化特征,作为建立分析方法的标准样品,采用标准曲线法通过相对强度与浓度的关联方式,建立钕铁硼样品中Nd、 Co、 B、 Dy、 Tb、 Pr、 Cu、 Al、 Ga九个元素的定量分析校准曲线;最后选取两个烧结钕铁硼试样,运用建立的定量分析方法完成九个元素的定量表征,分析时间小于30 s,其定量结果与ICP-OES法测定结果的比对,具有较好的一致性。运用激光诱导击穿光谱分析技术实现了对钕铁硼材料中多元素成分的直接、同时、快速定量表征,为钕铁硼材料的快速定量表征提供了新的技术思路和表征方法。

沿面放电光脉冲发展特征与临界击穿判据研究

绝缘沿面放电是引起高压开关柜中滑闪及电弧击穿的主要原因和前期阶段,准确有效地对绝缘异常爬电进行监测、跟踪和预警对保障设备安全运行非常关键。该文通过试验研究强垂直分量绝缘爬电的光脉冲阶段特征,并提出基于多波段光谱辐射强度信息的放电发展阶段划分方法和临界击穿判据,从而建立基于多波段光谱强度比值的放电跟踪预警方法。首先,搭建多波段单光子试验系统,采用自制多波段光学传感装置对沿面放电发展全过程跟踪测量,获得表征放电发展过程光谱比率的统计参量;其次,借助模糊聚类算法和支持向量机,构建放电发展临界特征空间边界,并对放电严重程度进行量化评估,结果表明该方法对放电阶段的正判率达到96.9%以上;最后,确立基于光谱比率的放电危险性主动预警逻辑,并开发了放电光脉冲跟踪预警系统,为开关柜放电和弧光监测的创新应用提供了参考。

沉析纤维尺寸和含量对间位芳纶纸性能的影响

使用不同目数的筛网对自制的Z沉析纤维进行筛分,将得到的不同尺寸的沉析纤维与间位芳纶短切纤维按一定质量比配抄成纸,制备间位芳纶纸;通过红外光谱、X射线衍射、扫描电镜及热失重、动态滤水分析对自制的Z沉析纤维的化学结构、热性能、动态滤水性能进行表征,并与进口的J沉析纤维对比;研究了沉析纤维的尺寸和含量对间位芳纶纸性能的影响。结果表明:Z沉析纤维与J沉析纤维均为膜状结构,化学结构基本一致,动态滤水性能及热性能相当;经30目或50目的筛网筛分后的沉析纤维可以与短切纤维更好地抱合,间位芳纶纸的抗张强度、断裂伸长率、撕裂度、击穿强度均达到较大值;间位芳纶纸的撕裂度随沉析纤维含量的增加逐渐降低,间位芳纶纸的抗张强度、断裂伸长率、击穿强度随沉析纤维含量的增加呈现先增后降的变化趋势,当沉析纤维质量分数为55%时,间位芳纶纸的抗张强度、断裂伸长率、击穿强度均达到最大值,分别为3.0 kN/m、5.50%、18.7 kV/mm。