CN108181294B - Raman spectrometer optical system - Google Patents
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- 238000001069 Raman spectroscopy Methods 0.000 title claims abstract description 35
- 230000003287 optical effect Effects 0.000 title claims abstract description 27
- 230000005540 biological transmission Effects 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims description 4
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- 230000005284 excitation Effects 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 3
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- 238000001919 Rayleigh scattering spectroscopy Methods 0.000 description 1
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
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Abstract
拉曼光谱仪光路系统，设有物镜、半反半透分束镜、透射光栅、全反射棱镜和角度补偿棱镜；物镜将准直的激光聚焦到样品上，收集散射光呈平行光束方式传输；半反半透分束镜将激光引入光路并让物镜收集到的散射光透过；透射光栅将收集到的散射光依据光栅衍射方程将不同波长的光以不同的空间角衍射；全反射棱镜固定在转动盘上，将光栅衍射的光引入全反射棱镜，转动全反射棱镜使激光瑞利线以恰好全内反射的角度入射，激光瑞利线全部被界面反射，拉曼信号光将以小于全内反射的角度入射而透过全反射棱镜，实现激光瑞利线的滤除；角度补偿棱镜与全反射棱镜组合成直平行六面体，信号光透过该角度补偿棱镜后空间角度将恢复到进入全反射棱镜前的角度。
The optical path system of the Raman spectrometer is equipped with an objective lens, a semi-reflective and semi-transparent beam splitter, a transmission grating, a total reflection prism and an angle compensation prism; the objective lens focuses the collimated laser onto the sample, collects the scattered light and transmits it in the form of a parallel beam; The anti-semi-transparent beam splitter introduces the laser into the optical path and allows the scattered light collected by the objective lens to pass through; the transmission grating diffracts the collected scattered light at different spatial angles according to the grating diffraction equation; the total reflection prism is fixed on On the rotating disk, the light diffracted by the grating is introduced into the total reflection prism. The total reflection prism is rotated to make the laser Rayleigh line incident at the angle of total internal reflection. All the laser Rayleigh lines are reflected by the interface, and the Raman signal light will be smaller than the total internal reflection angle. The angle of reflection is incident and passes through the total reflection prism to filter out the Rayleigh line of the laser; the angle compensation prism and the total reflection prism are combined to form a straight parallelepiped. After the signal light passes through the angle compensation prism, the spatial angle will return to the state of total reflection. The angle in front of the prism.
Description
技术领域Technical field
本发明涉及光谱检测，尤其是涉及拉曼光谱仪光路系统。The present invention relates to spectrum detection, and in particular to a Raman spectrometer optical path system.
背景技术Background technique
拉曼光谱学是通过检测分子的拉曼散射光来获取分子的振动、转动指纹信息而实现对分子结构的研究分析，广泛地应用于能源、生物，制药、食品安全等领域(1.伍林、等，光散射学报，2005年7月，第17卷，第二期，180-186页)。但是拉曼散射光的特点是信号弱(2.田中群，中国基础科学，2001年，第3卷，4-10页)，约为瑞利散射强度的10-6(拉曼光谱的检测器件通常需要低温制冷的高灵敏度CCD)，因此，收集到的散射光在进入光谱仪前必须滤除激光瑞利散射光(包括样品界面反射)，否则在未经衰减或者衰减系数不够高时，激光瑞利线将引起的CCD信号溢出甚至损坏。另外，激光瑞利散射光进入光谱仪将提高检测光谱杂散光背景水平，导致仪器检测灵敏度下降、谱图无法识别的问题，所以激光瑞利线的滤除是拉曼检测光路的关键环节，决定了拉曼光谱系统的光路类型。目前，主要有两种滤除激光瑞利线的方式，一种是多级光谱仪配合狭缝遮挡的空间滤波方式，另一种是使用光学介质镀膜或体布拉格光栅等全息元件的滤光片方式。Raman spectroscopy is to obtain the vibration and rotation fingerprint information of molecules by detecting the Raman scattered light of molecules to achieve research and analysis of molecular structures. It is widely used in energy, biology, pharmaceuticals, food safety and other fields (1. Wu Lin , et al., Journal of Light Scattering, July 2005, Volume 17, Issue 2, Pages 180-186). However, the characteristic of Raman scattered light is that the signal is weak (2. Tanaka Group, Basic Science of China, 2001, Volume 3, pp. 4-10), which is about 10-6 of the Rayleigh scattering intensity (detection device of Raman spectrum Usually a high-sensitivity CCD with low-temperature cooling is required. Therefore, the collected scattered light must filter out the laser Rayleigh scattered light (including sample interface reflection) before entering the spectrometer. Otherwise, the laser Rayleigh scattering light will not be attenuated or the attenuation coefficient is not high enough. Sharp lines will cause the CCD signal to overflow or even be damaged. In addition, laser Rayleigh scattered light entering the spectrometer will increase the background level of stray light in the detection spectrum, leading to problems such as a decrease in the detection sensitivity of the instrument and the inability to identify the spectrum. Therefore, the filtering of laser Rayleigh lines is a key link in the Raman detection optical path, which determines Optical path type of Raman spectroscopy system. Currently, there are two main ways to filter out laser Rayleigh lines. One is a spatial filtering method using a multi-level spectrometer combined with slit occlusion, and the other is a filter method using holographic elements such as optical media coatings or volume Bragg gratings. .
这两种方式都有明显的缺点：对于空间滤波方式，因为采用多级光谱仪导致结构复杂、仪器庞大、价格昂贵，而且光路中光学元件多，导致信号光的通光量显著减小，从而导致仪器检测灵敏度下降；对于滤光片方式，为了实现高OD的衰减值和高滤光陡度，滤光片波长通常无法调节或者只能在极小范围内可调，因此仪器无法适用于激发波长宽范围的连续可调，而且在紫外波段，波长越短，高OD值和高滤光陡度的滤光片越难实现，市场上提供的波长也很有限。Both methods have obvious shortcomings: for the spatial filtering method, the use of multi-stage spectrometers results in complex structures, large instruments, and expensive prices. Moreover, there are many optical components in the optical path, resulting in a significant reduction in the amount of signal light passing through, resulting in the failure of the instrument. The detection sensitivity decreases; for the filter method, in order to achieve high OD attenuation value and high filter steepness, the filter wavelength usually cannot be adjusted or can only be adjusted within a very small range, so the instrument cannot be applied to wide excitation wavelengths. The range is continuously adjustable, and in the ultraviolet band, the shorter the wavelength, the more difficult it is to achieve high OD value and high filter steepness filters, and the wavelengths available on the market are also very limited.
发明内容Contents of the invention
本发明的目的在于提供运用全内反射原理设计波长可调谐的滤光器，从而实现一种新型的全波长可调谐，结构紧凑的拉曼光谱仪光路系统。The purpose of the present invention is to provide a wavelength-tunable optical filter designed using the principle of total internal reflection, thereby realizing a new type of full-wavelength tunable and compact Raman spectrometer optical path system.
本发明设有：The invention is provided with:
一个物镜，该物镜将准直的激光聚焦到样品上，同时收集散射光呈平行光束方式传输；An objective lens that focuses the collimated laser onto the sample while collecting scattered light and transmitting it as a parallel beam;
一个半反半透分束镜，该半反半透分束镜将激光引入光路并让物镜收集到的散射光透过；A semi-reflective and semi-transparent beam splitter, which introduces the laser into the optical path and allows the scattered light collected by the objective lens to pass through;
一个透射光栅，该透射光栅将收集到的散射光依据光栅衍射方程将不同波长的光以不同的空间角衍射，所述散射光包括激光瑞利光和拉曼信号光；A transmission grating that diffracts the collected scattered light at different spatial angles according to the grating diffraction equation, and the scattered light includes laser Rayleigh light and Raman signal light;
一个全反射棱镜，该全反射棱镜固定在角度可调的转动盘上，将光栅衍射的光引入全反射棱镜，依据全反射棱镜玻璃材料的折射率n所决定的全内反射角度，转动全反射棱镜使激光瑞利线以恰好全内反射的角度入射，激光瑞利线全部被界面反射，而拉曼信号光将以小于全内反射的角度入射而透过全反射棱镜，实现激光瑞利线的滤除；A total reflection prism. The total reflection prism is fixed on an angle-adjustable rotating disk. The light diffracted by the grating is introduced into the total reflection prism. According to the total internal reflection angle determined by the refractive index n of the total reflection prism glass material, the total reflection prism is rotated. The prism causes the laser Rayleigh line to be incident at an angle just right for total internal reflection. The laser Rayleigh line is all reflected by the interface, while the Raman signal light will be incident at an angle smaller than total internal reflection and pass through the total reflection prism to realize the laser Rayleigh line. filtering;
一个角度补偿棱镜，该角度补偿棱镜与全反射棱镜组合成一个直平行六面体，信号光透过该角度补偿棱镜后空间角度将恢复到进入全反射棱镜前的角度。An angle compensation prism, which is combined with the total reflection prism to form a straight parallelepiped. After the signal light passes through the angle compensation prism, the spatial angle will be restored to the angle before entering the total reflection prism.
所述半反半透分束镜可采用半反半透全波段分束镜。The semi-reflective and semi-transparent beam splitter may be a semi-reflective and semi-transparent full-band beam splitter.
所述角度补偿棱镜与全反射棱镜的结构材料相同，以180°对称方式放置。The angle compensation prism is made of the same structural material as the total reflection prism and is placed in a 180° symmetrical manner.
本发明使用全内反射原理的滤光装置解决了激发波长全波段连续可调的问题，同时避免了使用多级光谱仪带来的结构复杂光通过量小的问题。The present invention uses a filter device based on the principle of total internal reflection to solve the problem of continuous adjustment of the excitation wavelength in the entire band, and at the same time avoids the problem of small light throughput caused by the use of a multi-stage spectrometer with a complicated structure.
与现有的技术相比，本发明具有以下突出的优点和技术效果：Compared with existing technology, the present invention has the following outstanding advantages and technical effects:
1、对于激光瑞利线的阻隔效果，由于本发明用了是全内反射的原理所以激光瑞利线被完全被阻隔，避免了激光瑞利线对检测器的干扰。而现有的商品化或实验室使用的介质膜滤光片方式的阻隔效果取决于滤光片的OD值，市场上优质的滤光片的OD值为4～6，对于拉曼仪器通常需要使用2片才能实现足够的阻隔效果。1. Regarding the blocking effect of the laser Rayleigh line, since the present invention uses the principle of total internal reflection, the laser Rayleigh line is completely blocked, avoiding the interference of the laser Rayleigh line on the detector. The blocking effect of existing commercial or laboratory dielectric film filters depends on the OD value of the filter. The OD value of high-quality filters on the market is 4 to 6, which is usually required for Raman instruments. Use 2 pieces to achieve sufficient blocking effect.
2、使用全内反射原理的滤光装置，可以通过转动棱镜改变入射角度从而改变全反射波长，因此波长全波段(包括紫外、可见、红外)连续可调，可适用于任意激光波长的瑞利线滤除，这一点介质膜滤光片是无法实现的，特别是在深紫外区，弥补了滤光片滤光陡度小，波长有限的问题。2. A filter device using the principle of total internal reflection can change the total reflection wavelength by changing the incident angle by rotating the prism. Therefore, the wavelength is continuously adjustable in the entire band (including ultraviolet, visible, and infrared) and can be applied to Rayleigh of any laser wavelength. Line filtering, which cannot be achieved with dielectric film filters, especially in the deep ultraviolet region, makes up for the problems of small filter steepness and limited wavelength of the filter.
3、对比使用多级光谱仪来实现波长可调谐方式，本发明具有检测灵敏度高、结构简单紧凑的特点。现有市场上，适用于激发波长可调谐的拉曼光谱仪是采用多级光谱仪方式，多级光谱仪使用光学元件多因而光学损耗大从而导致检测灵敏度下降，多级光谱仪系统结构也更为复杂庞大。3. Compared with using a multi-stage spectrometer to achieve wavelength tunability, the present invention has the characteristics of high detection sensitivity and simple and compact structure. In the current market, Raman spectrometers suitable for tunable excitation wavelengths use multi-stage spectrometers. Multi-stage spectrometers use many optical components, resulting in large optical losses, which leads to a decrease in detection sensitivity. The system structure of multi-stage spectrometers is also more complex and bulky.
4、透射光栅将准直光束衍射以后，可通过调整全反射棱镜角度，让不需要检测的波长的光束以大于全内反射角入射而被棱镜界面全反射阻挡住。转动透射光栅可实现全反射棱镜中恰好处于全反射角度的光束的波长连续可调。4. After the transmission grating diffracts the collimated beam, the angle of the total reflection prism can be adjusted so that the beam of the wavelength that does not need to be detected is incident at an angle greater than the total internal reflection and is blocked by total reflection at the prism interface. By rotating the transmission grating, the wavelength of the beam exactly at the total reflection angle in the total reflection prism can be continuously adjusted.
5、本发明使用一套光路系统通过转动光栅可适用于激光波长可调谐的拉曼光谱系统。5. The present invention uses an optical path system and can be applied to a Raman spectroscopy system with tunable laser wavelength by rotating the grating.
附图说明Description of the drawings
图1为本发明实施例的采用透射光栅的结构组成示意图。Figure 1 is a schematic diagram of the structural composition of a transmission grating according to an embodiment of the present invention.
图2为本发明实施例的采用反射光栅的结构组成示意图。FIG. 2 is a schematic diagram of the structural composition of a reflective grating according to an embodiment of the present invention.
具体实施方式Detailed ways
以下实施例将结合附图对本发明作进一步的说明。The following examples will further illustrate the present invention in conjunction with the accompanying drawings.
参见图1，标记1是拉曼散射激光光源，2是半反半透分束镜，3是物镜，4是待测样品，5是透射光栅，6是全反射棱镜，7是角度补偿棱镜，8是聚焦透镜，9是CCD。Referring to Figure 1, mark 1 is the Raman scattering laser light source, 2 is the semi-reflective and semi-transparent beam splitter, 3 is the objective lens, 4 is the sample to be measured, 5 is the transmission grating, 6 is the total reflection prism, 7 is the angle compensation prism, 8 is the focusing lens and 9 is the CCD.
拉曼散射激光光源1发射出的准直光束经半反半透分束镜2反射引入到物镜3里，经物镜3聚焦到待测样品4上，在焦点处，待测样品4散射出的激光瑞利线和拉曼信号光经显微物镜3收集后呈准直光束，通过半反半透分束镜2照射到透射光栅5上，经过透射光栅5衍射后的光束按波长以不同空间角出射，其中激光瑞利线波长比拉曼信号光波长短因而衍射角度较小，将这些波长按角度调制的光束照射到全反射棱镜6里，调整全反射棱镜6放置角度让激光瑞利线波长的光束在棱镜斜面上的入射角恰好处于全反射角度。拉曼信号光束因衍射角度大，所以入射角度比全反射角度小，因而可以透过角度补偿棱镜，角度补偿棱镜7以斜面平行方式放置在全反射棱镜6后以补偿全反射棱镜6带来的光束角度偏折，最后拉曼信号光光束经聚焦透镜8聚焦到CCD 9上，读出拉曼光谱。当激光波长发生变化时，通过转动光栅可以让激光光束始终处于全内反射角度，因而该光路系统可适用于激光波长连续可调的情况。The collimated beam emitted by the Raman scattering laser source 1 is reflected by the semi-transparent beam splitter 2 and introduced into the objective lens 3. It is focused on the sample 4 to be measured through the objective lens 3. At the focus, the sample 4 to be measured scatters The laser Rayleigh line and Raman signal light are collected by the microscope objective 3 and become a collimated beam, which is illuminated on the transmission grating 5 through the transflective beam splitter 2. The beam diffracted by the transmission grating 5 is distributed in different spaces according to the wavelength. Angle emission, in which the laser Rayleigh line wavelength is shorter than the Raman signal light wavelength, so the diffraction angle is smaller. The beams modulated by these wavelengths are irradiated into the total reflection prism 6, and the placement angle of the total reflection prism 6 is adjusted to make the laser Rayleigh line wavelength The incident angle of the light beam on the inclined surface of the prism is exactly at the angle of total reflection. The Raman signal beam has a large diffraction angle, so the incident angle is smaller than the total reflection angle, so it can pass through the angle compensation prism. The angle compensation prism 7 is placed behind the total reflection prism 6 in a bevel-parallel manner to compensate for the distortion caused by the total reflection prism 6. The angle of the beam is deflected, and finally the Raman signal light beam is focused on the CCD 9 through the focusing lens 8, and the Raman spectrum is read. When the laser wavelength changes, the laser beam can always be at the total internal reflection angle by rotating the grating, so this optical path system can be applied to situations where the laser wavelength is continuously adjustable.
图2是采用反射光栅时的光路系统，对比图1，光学元件的唯一不同是反射光栅代替了透射光栅，而光路的原理相同。在光路结构上，由光学元件拉曼散射激光光源1、半反半透分束镜2、物镜3和待测样品4组成的激发收集光路需要围绕光栅作一个180°的转动。Figure 2 shows the optical path system when a reflection grating is used. Compared with Figure 1, the only difference in the optical components is that the reflection grating replaces the transmission grating, and the principle of the optical path is the same. In terms of the optical path structure, the excitation and collection optical path composed of the optical element Raman scattering laser source 1, semi-reflective and semi-transparent beam splitter 2, objective lens 3 and sample to be measured 4 needs to rotate 180° around the grating.
本发明运用全内反射的原理来实现激光瑞利线滤除的拉曼光谱仪，激光作为拉曼散射光源由分束镜引入，经物镜聚焦到样品上，样品焦点处散射出的激光瑞利线和拉曼信号光经物镜收集，呈准直光束照射到光栅上，经过光栅衍射，光束按波长以不同空间角出射，再将这束波长经空间角调制的光束引入到棱镜里，调节棱镜和光栅的放置角度让处于激光瑞利线波长的光束恰好以全内反射角度入射到棱镜内的斜面上，而处于拉曼信号光波长的光束以小于全内反射角度入射到棱镜内的斜面上，因此激光瑞利线被在该斜面完全阻挡，而拉曼信号光则可以通过该界面，再经过聚焦透镜将拉曼信号光聚焦到CCD上而读出拉曼光谱。本发明用这种全新的方式解决拉曼散射中激光瑞利线的滤除问题，该方法通过角度调整可以滤除任意激光瑞利线，因而该光路系统可适用于任意波长激发的拉曼光谱仪。该光路系统结构相对简单紧凑，更具波长可调谐功能，在光谱检测上具有广阔的应用前景。The present invention uses the principle of total internal reflection to realize a Raman spectrometer that filters laser Rayleigh lines. The laser as a Raman scattering light source is introduced by a beam splitter and focused on the sample through the objective lens. The laser Rayleigh lines scattered at the focus of the sample The Raman signal light is collected by the objective lens and irradiated onto the grating in the form of a collimated beam. After diffraction by the grating, the beam emerges at different spatial angles according to the wavelength. Then the beam whose wavelength is modulated by the spatial angle is introduced into the prism, and the prism and The grating is placed at an angle such that the beam at the Rayleigh line wavelength of the laser is incident on the inclined surface in the prism at an angle of total internal reflection, while the beam at the wavelength of the Raman signal light is incident on the inclined surface in the prism at an angle smaller than the total internal reflection angle. Therefore, the laser Rayleigh line is completely blocked on this slope, and the Raman signal light can pass through this interface, and then focus the Raman signal light on the CCD through the focusing lens to read out the Raman spectrum. The present invention uses this brand-new method to solve the problem of filtering out laser Rayleigh lines in Raman scattering. This method can filter out any laser Rayleigh lines through angle adjustment, so the optical path system can be applied to Raman spectrometers excited at any wavelength. . The optical system has a relatively simple and compact structure, more wavelength tunable functions, and has broad application prospects in spectrum detection.
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