Name: quantitative analysis of vacuum induction melting by laser-induced breakdown spectroscopy
Uploaded: 2019-06-10T13:00:00
Description: Watch this Scientific Journal Video about Quantitative Analysis of Vacuum Induction Melting by Laser-induced Breakdown Spectroscopy at JoVE.com

本研究得到国家重点科学仪器和设备开发项目 (编号: 2014YQ120351)、中国科学院青年创新促进会 (2014136 号批准书) 和中国创新人才培养计划的资助。优先领域的创新团队 (第104 RA4051 号赠款)。

1. 标准样品的制备
注: 此步骤不是必需的。
<ol><li>准备原材料 (表 1)。要使100公斤的样品 #1, 在熔炉中加入12.82 千克铬、3.39 千克钼、4.79 千克铝、1.00 千克 Ti、0.60 千克铜和大约77.4 千克镍。在熔化过程中, 某些元素将被烧毁。最终成分由熔融温度、熔融时间和其他工作参数决定。成分测试显示了合金内每个元素的数量。</li>
	<li>在大约 1, 700°c 的温度下对每个标准...

<ol>
	<li>Radziemski, L., Cremers, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+brief+history+of+laser-induced+breakdown+spectroscopy:+From+the+concept+of+atoms+to+LIBS+2012.">A brief history of laser-induced breakdown spectroscopy: From the concept of atoms to LIBS 2012.</a> Spectrochimica Acta Part B: Atomic Spectroscopy. 87, 3-10 (2013).</li><li>El Haddad, J., Canioni, L., Bousquet, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Good+practices+in+LIBS+analysis:+Review+and+advices.">Good practices in LIBS analysis: Review and advices.</a> Spectrochimica Acta Part B: Atomic Spectroscopy. 101, 171-182 (2014).</li><li>Mueller, M., Gornushkin, I. 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F., Pasquini, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+compact+and+low+cost+laser+induced+breakdown+spectroscopic+system:+Application+for+simultaneous+determination+of+chromium+and+nickel+in+steel+using+multivariate+calibration.">A compact and low cost laser induced breakdown spectroscopic system: Application for simultaneous determination of chromium and nickel in steel using multivariate calibration.</a> Spectrochimica Acta Part B: Atomic Spectroscopy. 69, 20-24 (2012).</li><li>Peter, L., Sturm, V., Noll, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Liquid+steel+analysis+with+laser-induced+breakdown+spectrometry+in+the+vacuum+ultraviolet.">Liquid steel analysis with laser-induced breakdown spectrometry in the vacuum ultraviolet.</a> Applied Optics. 42 (30), 6199-6204 (2003).</li><li>Hubmer, G., Kitzberger, R., M&#246;rwald, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Application+of+LIBS+to+the+in-line+process+control+of+liquid+high-alloy+steel+under+pressure.">Application of LIBS to the in-line process control of liquid high-alloy steel under pressure.</a> Analytical and Bioanalytical Chemistry. 385 (2), 219-224 (2006).</li><li>Sun, L. X., Yu, H. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Automatic+estimation+of+varying+continuum+background+emission+in+laser-induced+breakdown+spectroscopy.">Automatic estimation of varying continuum background emission in laser-induced breakdown spectroscopy.</a> Spectrochimica Acta Part B: Atomic Spectroscopy. 64, 278-287 (2009).</li><li>Lin, X. M., Chang, P. H., Chen, G. H., Lin, J. J., Liu, R. X., Yang, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+melting+iron-based+alloy+temperature+on+carbon+content+observed+in+laser-induced+breakdown+spectroscopy.">Effect of melting iron-based alloy temperature on carbon content observed in laser-induced breakdown spectroscopy.</a> Plasma Science &amp; Technology. 17 (11), 933-937 (2015).</li><li>Rai, A. K., Yueh, F. Y., Singh, J. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Laser-induced+breakdown+spectroscopy+of+molten+aluminum+alloy.">Laser-induced breakdown spectroscopy of molten aluminum alloy.</a> Applied Optics. 42 (12), 2078-2084 (2003).</li><li>Hanson, C., Phongikaroon, S., Scott, J. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Temperature+effect+on+laser-induced+breakdown+spectroscopy+spectra+of+molten+and+solid+salts.">Temperature effect on laser-induced breakdown spectroscopy spectra of molten and solid salts.</a> Spectrochimica Acta Part B: Atomic Spectroscopy. 97, 79-85 (2014).</li><li>Darwiche, S., Benrabbah, R., Benmansour, M., Morvan, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Impurity+detection+in+solid+and+molten+silicon+by+laser+induced+breakdown+spectroscopy.">Impurity detection in solid and molten silicon by laser induced breakdown spectroscopy.</a> Spectrochimica Acta Part B: Atomic Spectroscopy. 74, 115-118 (2012).</li><li>Linstrom, P. J., Mallard, W. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=NIST+Chemistry+WebBook,+NIST+Standard+Reference+Database+Number+69.">NIST Chemistry WebBook, NIST Standard Reference Database Number 69.</a> National Institute of Standards and Technology. , 20899 (2018).</li></ol>

在元素分析方面, 常用的方法有 x 射线荧光 (XRF)、火花放电光学发射光谱法 (SD-OES)、原子吸收光谱 (AAS) 和电感耦合等离子体 (ICP)。这些方法主要适用于熔融合金的实验室和工业在线应用, 这是由这些技术的特点决定的, 是困难的。XRF 使用 x 射线冲击样品, SD-OES 在样品上产生火花。这两种方法的工作距离总是在几厘米的范围内。AAS 和 ICP 产生液体或粉末样品, 准备时间为几十分钟。这些方法不适合高...

激光诱导击穿光谱 (libs) 具有遥感、快速分析等独特功能, 无需样品制备, 为在线浓度测定1、2、 (三)有什么问题吗？尽管对 libs技术在不同领域的应用进行了 4、5、6 的研究, 但目前正在进行相当大的尝试, 以发展其在工业应用中的能力。
在工业过程中对熔融材料含量进行分析, 可以有效地提高产品质量, 是 LIBS 的一个有希望的发展方向。关于 libs 在工业领域的应用的实验研究结果已经报道, 例如关于氩氧液7、8、9、10、11、熔融的研究结果铝合金12、熔盐13和熔融硅14.这些材料大多存在于空气或辅助气体的环境中。然而, 真空感应熔炼 (VIM) 是 LIBS 实现加工控制的另一个良好应用领域。VIM 炉可以在1700°c 以上的温度下实现合金精炼的冶炼;它是精炼高纯度金属和合金 (如铁基或镍基合金、高纯度合金和清洁磁性合金) 的最常用方法。在熔炼过程中, 炉内压力始终在1-10 帕的区域内, 炉内空气的组成主要包括在熔炉样品或内壁吸收的空气以及一些氧化氧化物或氮化物金属。这些工作情况导致了相当不同的 LIBS 测量情况, 在空气中冶炼。本文报道了 LIBS 在 VIM 过程中对熔融合金进行分析的实验研究。
在熔炉中添加一个光学窗口, 用于激光烧蚀和辐射光检测。直径为80毫米的硅玻璃可用作窗口。发射激光和辐射光的收集使用相同的窗口;它是一种同轴光学结构, 聚焦于同一点。工作焦距约为1.8 米, 实验装置的对焦长度可从1.5 米调整到2.5 米。
基于工业在线分析的实用性, 在熔融合金成分分析中, 精度、可重复性和稳定性比低检测极限 (LOD) 更重要。选择了四通道线阵 CCD 光谱仪的技术路线, 光谱仪的光谱范围从190纳米到600纳米不等, 分辨率为 0.06 nm, 波长为200纳米。激光二极管泵浦 q 开关激光器 (内部构造) 用于烧蚀熔融合金, 输出能量为 100 mJ, 频率为 5 hz, FWHM 脉冲宽度为 20 ns, 工作波长为 1064 nm。其余部分将介绍 VIM libs 分析过程和实时测量, 然后介绍数据处理结果。

<table border="0" cellpadding="0" cellspacing="0" style="width:699px;" width="699">
	<colgroup>
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		<col />
		<col />
		<col />
	</colgroup>
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Laser source</td>
			<td style="width:135px;">Gklaser Co.,Ltd.</td>
			<td style="width:119px;"></td>
			<td style="width:229px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Molten alloy to be measured</td>
			<td style="width:135px;"></td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Smelting furnace</td>
			<td style="width:135px;">Tianyu Co.,Ltd.</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Spectrometer</td>
			<td style="width:135px;">Avantes</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">standard samples</td>
			<td style="width:135px;"></td>
			<td style="width:119px;"></td>
			<td>Well known of its composition</td>
		</tr>
	</tbody>
</table>

quantitative analysis of vacuum induction melting by laser-induced breakdown spectroscopy

真空感应熔炼是一种常用的精炼高纯度金属和合金的方法。传统上, 冶金中的标准过程控制涉及几个步骤, 包括绘制样品、冷却、切割、传输到实验室和分析。整个分析过程需要 3 0多分钟, 这阻碍了在线过程控制。激光感应击穿光谱分析是一种较好的在线分析方法, 由于快速、非接触、不需要样品制备, 能够满足感应熔炼的要求。该实验设施使用灯泵浦 q 开关激光器来烧蚀输出能量为 80 mJ 的熔化的钢液、5 Hz 的频率、20 NS 的 FWHM 脉冲宽度和 1, 064 纳米的工作波长。多通道线性电荷耦合器件 (CCD) 光谱仪用于实时测量发射光谱, 光谱范围为190至600纳米, 波长为200纳米的分辨率为 0.06 nm。该协议包括几个步骤: 标准合金样品制备和成分试验、标准样品的熔炼和激光击穿谱的确定, 以及每个元素浓度定量分析曲线的构建元素。为了实现未知样品的浓度分析, 还需要用相同的工艺对样品的光谱进行测量和处置。采用内部标准方法对熔融合金中所有主要元素的组成进行了定量分析。校准曲线表明, 大多数金属元素的检测极限从 20-250 ppm 不等。钛、钼、Nb、V 和铜等元素的浓度可以低于 100 ppm, 铬、铝、钴、铁、锰、C 和 Si 的浓度从 100-200 ppm 不等。某些校准曲线的 r2 可以超过0.94。

采用10个镍基合金样品 (#1 #10) 构造内部标准校准曲线。表 1列出了所有样品的成分。这些样品的元素浓度是正交设计的, 以避免信号干扰。用化学分析方法测量了所有样品中每个元素的浓度。
镍是内部标准元件。构造了铜、钛、钼、铝和铬的标定曲线。图 2到图 6显示了?...

Watch this Scientific Journal Video about Quantitative Analysis of Vacuum Induction Melting by Laser-induced Breakdown Spectroscopy at JoVE.com

Quantitative Analysis of Vacuum Induction Melting by Laser-induced Breakdown Spectroscopy

在真空感应熔炼过程中, 利用激光诱导击穿光谱仪对熔融合金的主要成分元素进行实时定量分析。

激光击穿光谱对真空感应熔融的定量分析

Vacuum induction melting is a popular method for refining high purity metal and alloys. Traditionally, standard process control in metallurgy involves ...

通过激光引起的分解光谱，实现了熔融合金成分的工业在线监测。通过该技术，可实时分析熔融合金的主要和微量元素。真空感应冶炼炉可以熔炼合金，这是最流行的合金精炼方法。对工业过程中熔融材料成分进行分析，可以有效地提高生产质量。LIBS 具有快速和远距离分析的优点。实现工业应用的在线成分分析是一种好的方法。演示程序将是新李和赵胜海，一个博士生和技术人员从我的实验室。要开始此过程，请分析标准样本并构建文本协议中概述的定量分析的校准曲线。然后将未知样品放入冶炼系统中。接下来打开激光发生器，使用脉冲宽度为 20 纳秒、频率为 5 赫兹、每个脉冲的能量为 90 毫焦耳，实现脉冲激光输出。打开光谱仪和频谱沉积软件，使用 190 到 600 纳米的光谱范围、200 纳米波长的分辨率为 0.06 纳米以及 10 毫秒的集成时间来确定频谱。在此之后，调整激光对焦位置，并对其进行优化，直到达到最强的频谱信号。确定激光分线光谱，注意每个激光脉冲产生一个频谱帧，并获取 20 帧的频谱并进行平均分析。等离子体光谱信号的强度是获得良好定量分析精度的重要因素。在我们的实验中，最高峰值的值应该超过10，000。对于频谱预处理，执行背景校正，如删除因破坏辐射而导致的背景效应，以执行频谱拟合。然后根据校准曲线的内部标准方法执行元素浓度分析。本研究中，使用10个镍基合金样品构建内部标准校准曲线。镍是内部标准元素，此处显示了铜、钛、硅、铝和铬的校准曲线。校准曲线都显示了元素浓度与峰值强度之间的近线性关系。所有信号峰都按信号强度、中央波长和洛伦茨拟合效果进行过滤。每个元素的检测限值是根据国际纯化学和应用化学联合会的标准计算的。实验结果表明，该技术可用于工业真空熔炼生产，可定量分析熔融合金的主要成分。

Research

JoVE Journal

Engineering

Measurement and Analysis of Atomic Hydrogen and Diatomic Molecular AlO, C2, CN, and TiO Spectra Following Laser-induced Optical Breakdown

Measurement and Analysis of Atomic Hydrogen and Diatomic Molecular AlO, C2, CN, and TiO Spectra Following Laser-induced Optical Breakdown

测量和原子氢和双原子分子ALO，C分析<sub&gt; 2</sub&gt;，CN和二氧化钛光谱承接激光诱导光学击穿

In this work, we present time-resolved measurements of atomic and diatomic spectra following laser-induced optical breakdown. A typical LIBS arrangement ...

科研

工程学

Laser-induced Breakdown Spectroscopy: A New Approach for Nanoparticle's Mapping and Quantification in Organ Tissue

激光诱导击穿光谱：对于纳米粒子的映射和定量的器官组织的新方法

Emission spectroscopy of laser-induced plasma was applied to elemental analysis of biological samples. Laser-induced breakdown spectroscopy (LIBS) ...

Investigating Single Molecule Adhesion by Atomic Force Spectroscopy

调查单分子粘附的原子力谱

Atomic force spectroscopy is an ideal tool to study molecules at surfaces and interfaces. An experimental protocol to couple a large variety of single ...

Laser-induced Forward Transfer for Flip-chip Packaging of Single Dies

激光诱导转发转移单人死于倒装芯片封装

Flip-chip (FC) packaging is a key technology for realizing high performance, ultra-miniaturized and high-density circuits in the micro-electronics ...

Seedless Growth of Bismuth Nanowire Array via Vacuum Thermal Evaporation

铋纳米线阵列通过真空热蒸发无核增长

Here a seedless and template-free technique is demonstrated to scalably grow bismuth nanowires, through thermal evaporation in high vacuum at RT. ...

Laser-induced Forward Transfer of Ag Nanopaste

银纳米糊膏的激光诱导正向传输

Over the past decade, there has been much development of non-lithographic methods1-3 for printing metallic inks or other functional materials. Many of ...

Free-form Light Actuators &#8212; Fabrication and Control of Actuation in Microscopic Scale

Free-form Light Actuators ÃƒÂ¢Ã¢â€šÂ¬Ã¢â‚¬Â Fabrication and Control of Actuation in Microscopic Scale

自由形式的光驱动器 - 制作和开动控制在微观尺度

Liquid crystalline elastomers (LCEs) are smart materials capable of reversible shape-change in response to external stimuli, and have attracted ...

Quantitative Hardness Measurement by Instrumented AFM-indentation

通过仪表AFM压痕硬度定量测量

In this work, a combination of amplitude-modulated non-contact atomic force microscopy and atomic force spectroscopy is applied for instrumented hardness ...

Fabrication of 1-D Photonic Crystal Cavity on a Nanofiber Using Femtosecond Laser-induced Ablation

1-D光子晶体空穴对纳米纤维使用飞秒激光诱导消融制造

We present a protocol for fabricating 1-D Photonic Crystal (PhC) cavities on subwavelength-diameter tapered optical fibers, optical nanofibers, using ...

Production and Characterization of Vacuum Deposited Organic Light Emitting Diodes

真空沉积有机发光二极管的生产与表征

A method for producing simple and efficient thermally-activated delayed fluorescence organic light-emitting diodes (OLEDs) based on guest-host or exciplex ...