CN107202787A - A kind of dipulse excites magnetic field space double constraints to strengthen the spectrum detection device of plasma - Google Patents
A kind of dipulse excites magnetic field space double constraints to strengthen the spectrum detection device of plasma Download PDFInfo
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Abstract
本发明公开一种双脉冲激发磁场空间双重约束增强等离子体的光谱检测装置,包括激光光源和样品台,所述样品台侧面设有用于在样品台周围形成磁场约束的磁性件;并设有覆盖样品台且透明的空间约束罩,该约束罩的内壁附有磁镜。本发明采用双脉冲激发、空间约束与磁场约束的三重作用,能够大大增强等离子体的光谱信号强度,具有密闭的检测环境,能够有效去除空气中其他元素对检测结果的干扰,提高检测精度。
The invention discloses a spectral detection device for double-pulse excitation magnetic field space double confinement enhanced plasma, which includes a laser light source and a sample stage, the side of the sample stage is provided with magnetic parts for forming magnetic field confinement around the sample stage; and a covering A sample stage and a transparent space confinement cover, and a magnetic mirror is attached to the inner wall of the confinement cover. The invention adopts the triple effect of double pulse excitation, space constraint and magnetic field constraint, can greatly enhance the spectral signal intensity of the plasma, has a closed detection environment, can effectively remove the interference of other elements in the air on the detection result, and improve the detection accuracy.
Description
技术领域technical field
本发明涉及激光诱导击穿光谱技术,特别涉及一种双脉冲激发磁场空间双重约束增强等离子体的光谱检测装置。The invention relates to laser-induced breakdown spectroscopy technology, in particular to a spectral detection device for double-pulse excitation magnetic field space double confinement enhanced plasma.
背景技术Background technique
激光诱导击穿光谱(Laser Induced Breakdown Spectroscopy,LIBS)是一种将高能激光脉冲聚焦在样品表面,激发样品表面产生等离子体的原子发射光谱的分析方法。由于该技术不需对样品进行复杂的预处理且能够实现无损检测,已成为目前快速检测物质成分的重要技术手段,在定性识别材料,定量分析物质成分等方面具有重要的应用。Laser Induced Breakdown Spectroscopy (LIBS) is an analytical method of atomic emission spectroscopy that focuses high-energy laser pulses on the surface of a sample and excites the surface of the sample to generate plasma. Since this technology does not require complex pretreatment of samples and can achieve non-destructive testing, it has become an important technical means for rapid detection of material components, and has important applications in qualitative identification of materials and quantitative analysis of material components.
与其他的光谱检测手段相比,LIBS技术具有样本无需预处理、检测速度快、检测元素多、能够实现远距离在线检测等优点,但目前仍存在检测灵敏度低、检测限高的技术瓶颈,限制了LIBS技术的进一步发展。如何增强LIBS信号的强度,提高LIBS探测技术的精确度和灵敏度是将LIBS技术向实用化方向推进的前提。目前的研究主要还局限于增加激光脉冲的个数,采用双脉冲或多脉冲的激发方式来增强光谱信号的强度,与单脉冲激发方式相比具有较好的效果但仍有进一步改进的空间。Compared with other spectral detection methods, LIBS technology has the advantages of no sample pretreatment, fast detection speed, multiple detection elements, and long-distance online detection. However, there are still technical bottlenecks such as low detection sensitivity and high detection limit. further development of LIBS technology. How to enhance the strength of LIBS signal and improve the accuracy and sensitivity of LIBS detection technology is the premise of advancing LIBS technology to the practical direction. Current research is mainly limited to increasing the number of laser pulses, using double-pulse or multi-pulse excitation to enhance the intensity of spectral signals, which has a better effect than single-pulse excitation, but there is still room for further improvement.
发明内容Contents of the invention
针对上述问题,本发明的目的在于提供一种利用双脉冲激发和磁场空间双重约束的方式增强等离子体的光谱检测装置。In view of the above problems, the purpose of the present invention is to provide a spectral detection device that utilizes double pulse excitation and magnetic field space double confinement to enhance plasma.
在本发明中,将从三个方面对等离子体的光谱信号进行增强:1.利用半球形腔构造对等离子体的空间约束,增强了等离子体的碰撞几率与碰撞强度;2.利用两个长直通电螺线管和半球形腔内壁磁镜的共同作用构造对等离子体的磁场约束,大大降低等离子体向外界的扩散速度;3.利用正交型双脉冲激发的方式,对预烧灼的等离子体进行二次激发,增强等离子体的原子光谱谱线强度。上述三个方面共同作用使等离子体的光谱信号大大增强,所述系统的检测限度与灵敏度也得以提升。In the present invention, the spectral signal of the plasma will be enhanced from three aspects: 1. Utilize the hemispherical cavity structure to confine the plasma to enhance the collision probability and collision intensity of the plasma; 2. Utilize two long The joint action structure of the straight-through electric solenoid and the magnetic mirror on the inner wall of the hemispherical cavity restricts the magnetic field of the plasma, greatly reducing the diffusion speed of the plasma to the outside; 3. Using the orthogonal double pulse excitation method, the pre-burned plasma The body undergoes secondary excitation to enhance the intensity of the atomic spectral line of the plasma. The combined effect of the above three aspects greatly enhances the spectral signal of the plasma, and the detection limit and sensitivity of the system are also improved.
本发明所采用的具体技术方案如下:The concrete technical scheme that the present invention adopts is as follows:
一种双脉冲激发磁场空间双重约束增强等离子体的光谱检测装置,包括激光光源和样品台,所述样品台侧面设有用于在样品台周围形成磁场约束的磁性件;A spectral detection device for double-pulse excitation of magnetic field space double confinement enhanced plasma, including a laser light source and a sample stage, the side of the sample stage is provided with magnetic parts for forming magnetic field confinement around the sample stage;
并设有覆盖样品台且透明的空间约束罩,该约束罩的内壁附有磁镜。A transparent space confinement cover covering the sample stage is provided, and a magnetic mirror is attached to the inner wall of the confinement cover.
本发明中,设有磁场约束和空间约束双重约束的样品台,其中磁性件为布置的样品台两两侧的通电螺线管,连接电压220V,频率50Hz的交流电,在样品台周围形成磁场约束;同时,样品台上罩有半密闭的半球形腔,腔内壁上附有磁镜,仅两束脉冲激光能够通过半球形腔烧灼激发样品产生等离子体,等离子体在半球形腔和磁镜的双重约束下,一部分等离子体向外扩散时经半球形腔反射,等离子体之间碰撞的强度增加,发光强度也随之增强,同时向外扩散的速度也由于空间和磁场的双重约束而大大减低,从而释放出更强的原子发射光谱信息。In the present invention, there is a sample stage with double constraints of magnetic field constraint and space constraint, wherein the magnetic parts are energized solenoids arranged on both sides of the sample stage, connected to an alternating current with a voltage of 220V and a frequency of 50Hz, forming a magnetic field constraint around the sample stage At the same time, the sample stage is covered with a semi-closed hemispherical cavity, and a magnetic mirror is attached to the inner wall of the cavity. Only two beams of pulsed lasers can excite the sample through the hemispherical cavity to generate plasma. Under the double constraints, a part of the plasma is reflected by the hemispherical cavity when it diffuses outwards, the intensity of the collision between the plasmas increases, and the luminous intensity also increases. At the same time, the speed of outward diffusion is also greatly reduced due to the dual constraints of space and magnetic field. , thus releasing stronger atomic emission spectral information.
作为优选的,所述的激光光源为两台Nd:YAG脉冲激光器倍频输出,其中一台Nd:YAG脉冲激光器发出的第一束预烧蚀激光脉冲波长为532nm,另一台Nd:YAG脉冲激光器发出的第二束激光脉冲波长为1064nm,其中,第一束预烧蚀激光脉冲采用经反光镜反射后垂直透镜聚焦方式,第二束激光脉冲采用直线透镜聚焦方式。As preferably, the laser light source is two Nd:YAG pulsed lasers frequency-multiplied output, wherein one Nd:YAG pulsed laser sends the first beam pre-ablation laser pulse wavelength is 532nm, another Nd:YAG pulsed laser The wavelength of the second laser pulse emitted by the laser is 1064nm. Among them, the first pre-ablation laser pulse is focused by a vertical lens after being reflected by a mirror, and the second laser pulse is focused by a linear lens.
进一步的,两束脉冲以正交型汇聚到样品表面,能量分别为50mJ和100mJ,第一束激光脉冲对样品进行预烧蚀后,第二束激光脉冲沿与样品表面平行的方向聚焦到第一束激光脉冲所激发的等离子体上对其再次激发增强。Further, two beams of pulses are converged to the sample surface in an orthogonal manner, with energies of 50mJ and 100mJ respectively. After the first laser pulse pre-ablates the sample, the second laser pulse is focused to the second laser pulse along the direction parallel to the sample surface. Re-excitation of the plasma excited by a laser pulse is enhanced.
本发明中,检测装置的实验环境为1个标准大气压,实验击穿环境为空气,激光光源为两台Nd:YAG脉冲激光器倍频输出,激光器的重复频率为10Hz。In the present invention, the experimental environment of the detection device is 1 standard atmospheric pressure, the experimental breakdown environment is air, the laser light source is two Nd:YAG pulsed lasers with frequency multiplied output, and the repetition frequency of the lasers is 10 Hz.
作为优选的,利用数字脉冲延时发生器同步控制两台Nd:YAG脉冲激光器的工作以及两脉冲之间的时序,两束激光脉冲之间的时间间隔为9μs。Preferably, a digital pulse delay generator is used to synchronously control the operation of two Nd:YAG pulse lasers and the timing between the two pulses, and the time interval between the two laser pulses is 9 μs.
作为优选的,设置由所述Nd:YAG脉冲激光器的调Q信号同步触发并进行信号采集的ICCD探测器,ICCD探测器能够将光敏元件上的光谱信息转换成相应比例的电荷量。Preferably, an ICCD detector synchronously triggered by the Q-switching signal of the Nd:YAG pulsed laser and used for signal acquisition is provided, and the ICCD detector can convert the spectral information on the photosensitive element into a corresponding proportion of charge.
作为优选的,还设有控制样品台进行平滑移动的位移控制台。位移控制台与样品圆台相连,为了避免激光束对样品表面造成同一部位的严重烧灼,位移控制台能够控制样品圆台的平滑移动,使激光脉冲烧灼在样品表面的不同位置上,对样品中表面不同区域的发射谱取平均值,能在一定程度上减少样品含量测量的误差。Preferably, a displacement console for controlling the smooth movement of the sample stage is also provided. The displacement console is connected with the sample round table. In order to avoid the laser beam from severely burning the same part of the sample surface, the displacement console can control the smooth movement of the sample round table, so that the laser pulse is burned at different positions on the sample surface, and the different surface of the sample is different. The average value of the emission spectrum of the area can reduce the error of the sample content measurement to a certain extent.
本发明具有的有益效果是:The beneficial effects that the present invention has are:
1)采用双脉冲激发、空间约束与磁场约束的三重作用,能够大大增强等离子体的光谱信号强度;1) The triple effect of double-pulse excitation, space confinement and magnetic field confinement can greatly enhance the spectral signal intensity of the plasma;
2)检测过程中由样品台上的半球形腔提供相对密闭的检测环境,能够有效去除空气中其他元素对检测结果的干扰,提高检测精度;2) During the detection process, the hemispherical cavity on the sample stage provides a relatively closed detection environment, which can effectively remove the interference of other elements in the air on the detection results and improve the detection accuracy;
3)装置可自由拆卸、组装,具有较大的灵活性。3) The device can be disassembled and assembled freely, with great flexibility.
附图说明Description of drawings
图1为双脉冲激发磁场空间双重约束增强等离子体的光谱检测装置图;Figure 1 is a diagram of a spectral detection device for double-pulse excitation magnetic field space double confinement enhanced plasma;
图2为所述检测系统的样品台。Fig. 2 is the sample stage of the detection system.
具体实施方式detailed description
下面结合实施例和附图来详细说明本发明,但本发明并不仅限于此。The present invention will be described in detail below in conjunction with the embodiments and accompanying drawings, but the present invention is not limited thereto.
如图1所示的双脉冲激发磁场空间双重约束增强等离子体的光谱检测装置,包括:ICCD检测器1,中阶梯光栅光谱仪2,计算机3,信号收集器4,样品台5,反光镜6,聚焦透镜7,Nd:YAG激光器8,数字延时脉冲发生器9和位移控制台10。As shown in Figure 1, the spectral detection device for double-pulse excitation magnetic field space double confinement enhanced plasma includes: ICCD detector 1, échelle grating spectrometer 2, computer 3, signal collector 4, sample stage 5, mirror 6, Focusing lens 7, Nd:YAG laser 8, digital delay pulse generator 9 and displacement console 10.
如图2所示,设有磁场约束和空间约束双重约束的样品台,包括长直通电螺线管51,内壁附有磁镜的半球形腔52,第一束激光脉冲53,待测样品54,样品圆台55,第二束激光脉冲56。As shown in Figure 2, there is a sample stage with double constraints of magnetic field constraint and space constraint, including a long straight-through electric solenoid 51, a hemispherical cavity 52 with a magnetic mirror on the inner wall, a first laser pulse 53, and a sample to be tested 54 , the sample circular stage 55 , the second laser pulse 56 .
本实施例中的双脉冲激发磁场空间双重约束增强等离子体的光谱检测装置,具体操作步骤如下:The specific operation steps of the spectral detection device for double-pulse excitation magnetic field space double confinement enhanced plasma in this embodiment are as follows:
第一步,将长直通电螺线管51接通电压220V,频率50Hz的交流电源,在样品台上方产生交变磁场,半球形腔自身阻碍了等离子体向外界扩散,同时其内壁上的磁镜使交变磁场对等离子体的约束力进一步提升。In the first step, the long straight-through electric solenoid 51 is connected to an AC power supply with a voltage of 220V and a frequency of 50Hz, and an alternating magnetic field is generated above the sample stage. The mirror further enhances the binding force of the alternating magnetic field to the plasma.
第二步,由Nd:YAG激光器8发射的第一束激光脉冲53经反射镜6和透镜7后聚焦在样品表面并对样品进行预烧蚀,第二束激光脉冲56沿与样品表面平行的方向经透镜聚焦后对等离子体进行二次激发,数字脉冲延时发生器9同步控制两台激光器的工作以及两脉冲之间的时序,两束激光脉冲之间的时间间隔为9μs。In the second step, the first laser pulse 53 emitted by the Nd:YAG laser 8 is focused on the sample surface after the reflector 6 and the lens 7, and the sample is pre-ablated, and the second laser pulse 56 is parallel to the sample surface. After the direction is focused by the lens, the plasma is re-excited. The digital pulse delay generator 9 synchronously controls the work of the two lasers and the timing between the two pulses. The time interval between the two laser pulses is 9 μs.
第三步,位移控制台10与样品圆台55相连,为了避免激光束对样品表面造成同一部位的严重烧灼,位移控制台10能够控制样品圆台的平滑移动,使激光脉冲烧灼在样品表面的不同位置上,对样品中表面不同区域的发射谱取平均值,能在一定程度上减少样品含量测量的误差。In the third step, the displacement console 10 is connected with the sample circular table 55. In order to prevent the laser beam from severely burning the same part of the sample surface, the displacement console 10 can control the smooth movement of the sample circular table, so that the laser pulses can be burned at different positions on the sample surface. On the other hand, averaging the emission spectra of different regions of the surface of the sample can reduce the error of sample content measurement to a certain extent.
第四步,等离子体所产生的光谱信号由信号收集器4收集,经光纤传输至配有ICCD检测器的中阶梯光栅光谱仪,利用计算机根据现有模型库对采集的光谱信息进行存储和分析。In the fourth step, the spectral signal generated by the plasma is collected by the signal collector 4, and transmitted to the échelle spectrometer equipped with an ICCD detector through the optical fiber, and the collected spectral information is stored and analyzed by the computer according to the existing model library.
以上所述仅为本发明的较佳实施举例,并不用于限制本发明,凡在本发明精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。The above descriptions are only examples of the preferred implementation of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection scope of the present invention within.
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CN112945936A (en) * | 2021-01-28 | 2021-06-11 | 西安电子科技大学 | Liquid sample spectral measurement method and device based on laser plasma self-constraint |
CN114226279A (en) * | 2021-12-13 | 2022-03-25 | 欧冶云商股份有限公司 | Automatic detecting and sorting device for alloy content of steel waste and inferior materials |
CN114509424A (en) * | 2021-12-29 | 2022-05-17 | 清华大学 | System for enhancing the intensity and repeatability of plasma spectra and methods of using the same |
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