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CN105067571B - A kind of Laser induced plasma spectroscopy intensifier - Google Patents

A kind of Laser induced plasma spectroscopy intensifier Download PDF

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CN105067571B
CN105067571B CN201510506041.2A CN201510506041A CN105067571B CN 105067571 B CN105067571 B CN 105067571B CN 201510506041 A CN201510506041 A CN 201510506041A CN 105067571 B CN105067571 B CN 105067571B
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laser
cavity
focusing lens
diverging
inert gas
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CN105067571A (en
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阳建宏
曹康
徐金梧
杨德斌
黎敏
孟凡星
李晓萌
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University of Science and Technology Beijing USTB
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Abstract

本发明提供一种激光诱导等离子体光谱增强装置,属于激光等离子体光谱检测领域。该装置包括发散腔、聚焦透镜、汇聚腔、光纤探头、底座、可调样品台、等离子体、惰性气体接口和激光滤波片,发散腔、聚焦透镜、底座和激光滤波片构成封闭空间,惰性气体接口接在发散腔上,样品放在可调样品台上,可调样品台安装在底座上,聚焦透镜另一侧为汇聚腔,光纤探头在汇聚腔上,等离子体为激光激发样品产生。该装置与脉冲激光器、光路系统、光谱仪、惰性气体保护系统共同实现激光诱导击穿光谱技术的光谱增强。该装置增强了等离子体光谱,减弱了背景光干扰,结构简单,成本低,无需消耗其他形式的能源,操作简便。

The invention provides a laser-induced plasma spectrum enhancement device, which belongs to the field of laser plasma spectrum detection. The device includes a diverging cavity, focusing lens, converging cavity, fiber optic probe, base, adjustable sample stage, plasma, inert gas interface and laser filter. The diverging cavity, focusing lens, base and laser filter form a closed space, and the inert gas The interface is connected to the divergent cavity, the sample is placed on the adjustable sample stage, and the adjustable sample stage is installed on the base. The device, together with a pulsed laser, an optical system, a spectrometer, and an inert gas protection system, realizes the spectral enhancement of laser-induced breakdown spectroscopy. The device enhances the plasma spectrum, weakens background light interference, has simple structure, low cost, does not need to consume other forms of energy, and is easy to operate.

Description

一种激光诱导等离子体光谱增强装置A laser-induced plasma spectral enhancement device

技术领域technical field

本发明涉及激光等离子体光谱检测领域,特别是指一种激光诱导等离子体光谱增强装置。The invention relates to the field of laser plasma spectrum detection, in particular to a laser-induced plasma spectrum enhancement device.

背景技术Background technique

激光诱导击穿光谱(Laser-induced breakdown spectroscopy,简称为LIBS)是采用聚焦的高能量脉冲激光入射到样品的表面产生等离子体,通过分析该等离子体的辐射光谱,从而推导出样品的元素组成成分及含量。LIBS技术具有很多显著优点:能够探测所有元素,可同时检测多种元素,无需真空,样品制备简单或无需制备,被分析样品几乎无损,可以实时分析,原位探测和远程探测等。但是,探测极限差、分析精度低,导致LIBS的探测灵敏度低已成为该技术发展的瓶颈问题。针对以上LIBS的不足,通过增强LIBS的光谱强度,改善LIBS检测的灵敏度和精度,可以提高LIBS的探测灵敏度。大量的研究工作结果表明,磁约束装置、空间约束装置、双脉冲激发均能明显提高激光诱导等离子体光谱谱线强度。Laser-induced breakdown spectroscopy (LIBS for short) uses a focused high-energy pulsed laser incident on the surface of the sample to generate plasma. By analyzing the radiation spectrum of the plasma, the elemental composition of the sample can be deduced. and content. LIBS technology has many significant advantages: it can detect all elements, multiple elements can be detected at the same time, no vacuum is needed, sample preparation is simple or no preparation is required, the analyzed sample is almost non-destructive, real-time analysis, in situ detection and remote detection, etc. However, the poor detection limit and low analysis precision lead to the low detection sensitivity of LIBS, which has become the bottleneck of the development of this technology. For the above shortcomings of LIBS, the detection sensitivity of LIBS can be improved by enhancing the spectral intensity of LIBS and improving the sensitivity and precision of LIBS detection. A large number of research results have shown that magnetic confinement devices, spatial confinement devices, and double-pulse excitation can significantly increase the intensity of laser-induced plasma spectral lines.

但磁约束装置结构复杂,安装不便,效率较低,一般只能放大2-3倍,需要消耗电能。双脉冲激发方式放大效果较好,但成本较高,光路搭建复杂。常用的空间约束装置功能单一,不能直接采集光谱,装置搭建复杂,放大效果最好的半球形能增强12倍。However, the structure of the magnetic confinement device is complicated, it is inconvenient to install, and the efficiency is low. Generally, it can only be enlarged by 2-3 times, and it needs to consume electric energy. The amplification effect of the double-pulse excitation method is better, but the cost is high and the optical path is complicated. Commonly used spatial confinement devices have a single function, cannot directly collect spectra, and the device is complex to build. The hemispherical shape with the best amplification effect can be enhanced by 12 times.

发明内容Contents of the invention

本发明要解决的技术问题是提供一种激光诱导等离子体光谱增强装置。The technical problem to be solved by the present invention is to provide a laser-induced plasma spectrum enhancement device.

该装置包括发散腔、聚焦透镜、汇聚腔、光纤探头、底座、可调样品台、惰性气体接口和激光滤波片,其中,发散腔、聚焦透镜、底座和激光滤波片组成封闭空间,惰性气体接口接在发散腔上,聚焦透镜另一侧连接汇聚腔,汇聚腔与发散腔通过螺母连接固定,光纤探头在汇聚腔上,可调样品台安装在底座上,可调样品台上放置样品,激光激发样品产生等离子体。The device includes a diverging cavity, a focusing lens, a converging cavity, an optical fiber probe, a base, an adjustable sample stage, an inert gas interface, and a laser filter. Connected to the diverging cavity, the other side of the focusing lens is connected to the converging cavity, the converging cavity and the diverging cavity are connected and fixed by nuts, the fiber optic probe is on the converging cavity, the adjustable sample stage is installed on the base, and the sample is placed on the adjustable sample stage. Excite the sample to generate plasma.

发散腔能将等离子体球面发射出的光谱反射成平行光,经过聚焦透镜之后,将光线聚焦在汇聚腔的光纤探头上,相比传统收光方式接收少量的光谱,本装置接收了左半球反射和右半球直射的大部分光谱,实现增大收光面积的作用,从而大大增强光谱强度。The diverging cavity can reflect the spectrum emitted by the plasma sphere into parallel light. After passing through the focusing lens, the light is focused on the fiber optic probe of the converging cavity. Compared with the traditional light receiving method to receive a small amount of spectrum, this device receives the left hemisphere reflection Most of the spectrum directly irradiated by the right hemisphere realizes the effect of increasing the light-receiving area, thereby greatly enhancing the spectral intensity.

激发出的等离子体被约束发散腔与聚焦透镜以及底座、激光滤波片围成的封闭空间内,伴随该等离子体产生的冲击波将以超音速向外传播,当其传播到该封闭空腔内壁时在内壁上发生反射,反射回来的冲击波将压缩等离子体,被压缩后的等离子体体积变小,等离子内部温度增加并变得更亮,从而释放出更强的原子、离子光谱。The excited plasma is confined to the closed space surrounded by the diverging cavity, the focusing lens, the base, and the laser filter. The shock wave generated with the plasma will propagate outward at supersonic speed. When it propagates to the inner wall of the closed cavity Reflection occurs on the inner wall, and the reflected shock wave will compress the plasma. The volume of the compressed plasma becomes smaller, and the internal temperature of the plasma increases and becomes brighter, thereby releasing a stronger spectrum of atoms and ions.

发散腔、聚焦透镜以及底座、激光滤波片围成的封闭空间内通过惰性气体接口充入惰性气体,隔离空气,避免了空气中元素成分的干扰,减小了空气对测量结果的干扰。Inert gas is filled into the closed space surrounded by diverging cavity, focusing lens, base and laser filter through the inert gas interface to isolate the air, avoid the interference of elemental components in the air, and reduce the interference of air on the measurement results.

激光滤波片只能允许与激光波长相同的光进入,阻挡其他波长的光进入装置,从而没有外界背景光干扰,增大了信噪比。The laser filter can only allow the light of the same wavelength as the laser to enter, and block the light of other wavelengths from entering the device, so that there is no external background light interference and the signal-to-noise ratio is increased.

发散腔的焦点与聚焦透镜的左侧焦点位置重合,聚焦透镜的右侧焦点在汇聚腔的光纤探头上,实现了左侧发散腔反射出的光经过聚焦透镜的作用后能够准确的聚焦在汇聚腔的光纤探头上。The focal point of the diverging cavity coincides with the left focal point of the focusing lens, and the right focus of the focusing lens is on the fiber optic probe of the converging cavity, so that the light reflected from the left diverging cavity can be accurately focused on the converging lens after passing through the focusing lens. cavity fiber optic probe.

底座安装有可调样品台,能够调整样品高度,通过调节可调样品台能控制样品上表面与发散腔焦点的距离,即激光激发样品产生的等离子体能始终位于焦点位置,并且可使样品旋转一定角度,实现样品多个位置的测量。The base is equipped with an adjustable sample stage, which can adjust the height of the sample. By adjusting the adjustable sample stage, the distance between the upper surface of the sample and the focal point of the divergent cavity can be controlled, that is, the plasma generated by the sample excited by the laser can always be at the focal point, and the sample can be rotated by a certain amount. Angle, to achieve the measurement of multiple positions of the sample.

发散腔内壁使用包括但不限于嵌入某种曲线的凹面镜,或在发散腔内壁通过镀膜的方式反射等离子体光谱。The inner wall of the diverging cavity includes but is not limited to a concave mirror embedded in a certain curve, or the plasma spectrum is reflected by coating the inner wall of the diverging cavity.

该装置与脉冲激光器、光路系统、光谱仪、惰性气体保护系统共同实现激光诱导击穿光谱技术的光谱增强。The device, together with a pulsed laser, an optical system, a spectrometer, and an inert gas protection system, realizes the spectral enhancement of laser-induced breakdown spectroscopy.

本发明的上述技术方案的有益效果如下:The beneficial effects of above-mentioned technical scheme of the present invention are as follows:

1、结合空间约束和光谱反射后再汇聚能使光谱强度大大增强;1. Combined with spatial constraints and spectral reflection, reconvergence can greatly enhance the spectral intensity;

2、装置腔内部密封,几乎没有背景光干扰,且有惰性气体的保护,信噪比高;2. The interior of the device cavity is sealed, there is almost no background light interference, and it is protected by inert gas, and the signal-to-noise ratio is high;

3、装置使用方便,可调节样品高度和位置,汇聚腔安装光纤探头方便光谱采集;3. The device is easy to use, the height and position of the sample can be adjusted, and the optical fiber probe is installed in the converging cavity to facilitate spectrum collection;

4、装置成本低,无需消耗其他能源。4. The installation cost is low, and no other energy consumption is required.

附图说明Description of drawings

图1为本发明的激光诱导等离子体光谱增强装置结构示意图;Fig. 1 is a schematic structural diagram of a laser-induced plasma spectral enhancement device of the present invention;

图2为本发明的激光诱导等离子体光谱增强装置安装关系示意图;Fig. 2 is a schematic diagram of the installation relationship of the laser-induced plasma spectral enhancement device of the present invention;

图3为本发明的激光诱导等离子体光谱增强装置内部光路示意图。Fig. 3 is a schematic diagram of the internal optical path of the laser-induced plasma spectrum enhancement device of the present invention.

其中:1-发散腔;2-聚焦透镜;3-汇聚腔;4-光纤探头;5-底座;6-可调样品台;7-样品;8-等离子体;9-惰性气体接口;10-激光滤波片。Among them: 1- diverging cavity; 2- focusing lens; 3- converging cavity; 4- fiber optic probe; 5- base; 6- adjustable sample stage; 7- sample; 8- plasma; 9- inert gas interface; 10- Laser filters.

具体实施方式detailed description

为使本发明要解决的技术问题、技术方案和优点更加清楚,下面将结合附图及具体实施例进行详细描述。In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following will describe in detail with reference to the drawings and specific embodiments.

本发明针对现有的LIBS增强装置灵敏度差、装置复杂等问题,提供一种激光诱导等离子体光谱增强装置。The invention provides a laser-induced plasma spectrum enhancement device aiming at the problems of poor sensitivity and complex device of the existing LIBS enhancement device.

如图1所示,该装置包括发散腔1、聚焦透镜2、汇聚腔3、光纤探头4、底座5、可调样品台6、惰性气体接口9和激光滤波片10,发散腔1、聚焦透镜2、底座5和激光滤波片10组成封闭空间,惰性气体接口9接在发散腔1上,聚焦透镜2另一侧连接汇聚腔3,汇聚腔3与发散腔1通过螺母连接固定,光纤探头4在汇聚腔3上,可调样品台6安装在底座5上,可调样品台6上放置样品7,激光激发样品7产生等离子体8。As shown in Figure 1, the device includes diverging cavity 1, focusing lens 2, converging cavity 3, fiber optic probe 4, base 5, adjustable sample stage 6, inert gas interface 9 and laser filter 10, diverging cavity 1, focusing lens 2. The base 5 and the laser filter 10 form a closed space. The inert gas interface 9 is connected to the diverging cavity 1. The other side of the focusing lens 2 is connected to the converging cavity 3. The converging cavity 3 and the diverging cavity 1 are connected and fixed by nuts. The optical fiber probe 4 On the converging cavity 3 , an adjustable sample stage 6 is installed on the base 5 , and a sample 7 is placed on the adjustable sample stage 6 , and a laser excites the sample 7 to generate a plasma 8 .

如图2所示,该装置与脉冲激光器、光路系统、光谱仪、惰性气体保护系统共同实现激光诱导击穿光谱技术的光谱增强。As shown in Figure 2, the device, together with the pulsed laser, optical path system, spectrometer, and inert gas protection system, realizes the spectral enhancement of laser-induced breakdown spectroscopy.

使用前将聚焦透镜2置于发散腔1与汇聚腔3中间的安装位中,两腔通过螺母连接固定,夹紧聚焦透镜2使之成为整体。将样品7放置于底座5的可调样品台6上,调整可调样品台6使样品7上表面与底座5上表面距离合适,这样就能保证等离子体8在发散腔内的凹面镜焦点处。搭建好脉冲激光器、光谱仪,外部光路系统后,调节外部光路使激光聚焦在样品7表面。最后将连接好的发散腔1、聚焦透镜2、汇聚腔3整体置于底座5上方,使之贴合紧密成为整体。至此装置安装完成,接下来将惰性气体通过惰性气体接口9接入发散腔1,光谱仪的光纤连接汇聚腔3即可。Before use, the focusing lens 2 is placed in the installation position between the diverging cavity 1 and the converging cavity 3, and the two cavities are connected and fixed by nuts, and the focusing lens 2 is clamped to make it integrated. Place the sample 7 on the adjustable sample stage 6 of the base 5, adjust the adjustable sample stage 6 so that the distance between the upper surface of the sample 7 and the upper surface of the base 5 is appropriate, so that the plasma 8 can be ensured at the focal point of the concave mirror in the diverging cavity . After building the pulse laser, spectrometer, and external optical path system, adjust the external optical path to focus the laser on the surface of the sample 7 . Finally, the connected diverging cavity 1, focusing lens 2, and converging cavity 3 are placed on the base 5 as a whole, so that they are tightly bonded to form a whole. At this point, the installation of the device is completed, and then the inert gas is connected to the diverging cavity 1 through the inert gas interface 9, and the optical fiber of the spectrometer is connected to the converging cavity 3.

如图3所示,实验时脉冲激光通过外部光路系统聚焦后穿过发散腔1上的激光滤波片10打在样品7上,光谱经发散腔1内壁的反射成平行光射向聚焦透镜2,经过聚焦透镜2的聚焦后在汇聚腔3底部的光纤探头5上形成焦点,将左侧半球大面积的反射光线和右边球的直射光线汇集到光纤探头5大大增强了光谱强度。另一方面激发出的等离子体8被约束在发散腔1、聚焦透镜2以及底座5围成的封闭空间内,伴随该等离子体8产生的冲击波将以超音速向外传播,当其传播到该封闭空腔内壁时在内壁上发生反射,反射回来的冲击波将压缩等离子体8,被压缩后的等离子体8体积变小,等离子内部温度增加并变得更亮,从而释放出更强的原子、离子光谱。As shown in Figure 3, during the experiment, the pulsed laser is focused by the external optical path system and then passes through the laser filter 10 on the diverging cavity 1 and hits the sample 7, and the spectrum is reflected by the inner wall of the diverging cavity 1 into parallel light and directed to the focusing lens 2. After focusing by the focusing lens 2, a focus is formed on the fiber optic probe 5 at the bottom of the converging cavity 3, and the large-area reflected light from the left hemisphere and the direct light from the right sphere are collected into the fiber optic probe 5 to greatly enhance the spectral intensity. On the other hand, the excited plasma 8 is confined in the closed space enclosed by the diverging cavity 1, the focusing lens 2 and the base 5, and the shock wave produced with the plasma 8 will propagate outward at supersonic speed. When the inner wall of the cavity is closed, reflection occurs on the inner wall, and the reflected shock wave will compress the plasma 8, and the volume of the compressed plasma 8 becomes smaller, and the internal temperature of the plasma increases and becomes brighter, thereby releasing stronger atoms, ion spectrum.

以上所述是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明所述原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。The above description is a preferred embodiment of the present invention, it should be pointed out that for those of ordinary skill in the art, without departing from the principle of the present invention, some improvements and modifications can also be made, these improvements and modifications It should also be regarded as the protection scope of the present invention.

Claims (7)

1.一种激光诱导等离子体光谱增强装置,其特征在于:包括发散腔(1)、聚焦透镜(2)、汇聚腔(3)、光纤探头(4)、底座(5)、可调样品台(6)、惰性气体接口(9)和激光滤波片(10),发散腔(1)、聚焦透镜(2)、底座(5)和激光滤波片(10)组成封闭空间,惰性气体接口(9)接在发散腔(1)上,聚焦透镜(2)一侧连接汇聚腔(3),汇聚腔(3)与发散腔(1)通过螺母连接固定,光纤探头(4)在汇聚腔(3)上,可调样品台(6)安装在底座(5)上,可调样品台(6)上放置样品(7),激光激发样品(7)产生等离子体(8)。1. A laser-induced plasma spectral enhancement device, characterized in that: comprising a diverging cavity (1), a focusing lens (2), a converging cavity (3), an optical fiber probe (4), a base (5), an adjustable sample stage (6), the inert gas interface (9) and the laser filter (10), the divergent cavity (1), the focusing lens (2), the base (5) and the laser filter (10) form a closed space, and the inert gas interface (9 ) is connected to the diverging cavity (1), one side of the focusing lens (2) is connected to the converging cavity (3), the converging cavity (3) and the diverging cavity (1) are connected and fixed by nuts, and the optical fiber probe (4) is connected to the converging cavity (3) ), the adjustable sample stage (6) is installed on the base (5), the sample (7) is placed on the adjustable sample stage (6), and the laser excites the sample (7) to generate plasma (8). 2.根据权利要求1所述的一种激光诱导等离子体光谱增强装置,其特征在于:所述发散腔(1)将等离子体(8)球面发射出的光谱反射成平行光,经过聚焦透镜(2)之后,将光线聚焦在汇聚腔(3)的光纤探头(4)上。2. A kind of laser-induced plasma spectrum enhancement device according to claim 1, characterized in that: said divergence cavity (1) reflects the spectrum emitted by the spherical surface of plasma (8) into parallel light, and passes through the focusing lens ( 2) After that, focus the light on the fiber optic probe (4) of the converging cavity (3). 3.根据权利要求1所述的一种激光诱导等离子体光谱增强装置,其特征在于:所述发散腔(1)、聚焦透镜(2)以及底座(5)、激光滤波片(10)围成的封闭空间内通过惰性气体接口(9)充入惰性气体,隔离空气。3. A kind of laser-induced plasma spectrum enhancement device according to claim 1, characterized in that: said diverging cavity (1), focusing lens (2), base (5), and laser filter (10) are surrounded by Fill the closed space with inert gas through the inert gas interface (9) to isolate the air. 4.根据权利要求1所述的一种激光诱导等离子体光谱增强装置,其特征在于:所述激光滤波片(10)只能允许与激光波长相同的光进入,阻挡其他波长的光进入装置。4. A laser-induced plasma spectrum enhancement device according to claim 1, characterized in that: the laser filter (10) can only allow light with the same wavelength as the laser to enter, and prevent light with other wavelengths from entering the device. 5.根据权利要求1所述的一种激光诱导等离子体光谱增强装置,其特征在于:所述发散腔(1)的焦点与聚焦透镜(2)的左侧焦点位置重合,聚焦透镜(2)的右侧焦点在汇聚腔(3)的光纤探头(4)上。5. A kind of laser-induced plasma spectrum enhancement device according to claim 1, characterized in that: the focal point of the diverging cavity (1) coincides with the left focus position of the focusing lens (2), and the focusing lens (2) The right focus of is on the fiber optic probe (4) of the converging cavity (3). 6.根据权利要求1所述的一种激光诱导等离子体光谱增强装置,其特征在于:通过调节可调样品台(6)的高度,控制样品(7)上表面与发散腔(1)焦点的距离。6. A kind of laser-induced plasma spectrum enhancement device according to claim 1, characterized in that: by adjusting the height of the adjustable sample stage (6), the distance between the upper surface of the sample (7) and the focal point of the diverging cavity (1) is controlled distance. 7.根据权利要求1所述的一种激光诱导等离子体光谱增强装置,其特征在于:所述发散腔(1)内壁使用嵌入某种曲线的凹面镜,或在发散腔(1)内壁通过镀膜的方式反射等离子体光谱。7. A laser-induced plasma spectral enhancement device according to claim 1, characterized in that: the inner wall of the diverging cavity (1) uses a concave mirror embedded with a certain curve, or the inner wall of the diverging cavity (1) is coated way to reflect the plasma spectrum.
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