CN113063752B - Double-beam-splitting near infrared spectrometer based on supercontinuum laser - Google Patents
Double-beam-splitting near infrared spectrometer based on supercontinuum laser Download PDFInfo
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
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- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
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- G01N2201/064—Stray light conditioning
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Abstract
The invention discloses a bicontinuous spectrum laser-based dual-beam near infrared spectrometer, which comprises a bicontinuous spectrum laser, a front beam splitter, a rear beam splitter and a detector which are sequentially arranged according to an optical path, wherein the front beam splitter is arranged in front of a sample, and the rear beam splitter is arranged behind the sample. The front-end beam splitter and the rear-end beam splitter are arranged in front of and behind the sample, so that the repeatability and the stability of the instrument can be improved, light spots irradiated on the sample are smaller, the energy is stronger, the fault analysis and the detection of the sample can be performed, and the using amount of precious samples is saved.
Description
Technical Field
The invention relates to the technical field of infrared spectrum analysis, in particular to a double-beam-splitting near infrared spectrometer based on a supercontinuum laser.
Background
Because the sample does not need to be processed basically during analysis, the sample is not destroyed and consumed, the sample does not pollute the environment, the near infrared spectrum analysis technology is a typical representative of a green analysis instrument, and the near infrared spectrum analysis technology is increasingly accepted and applied as a nondestructive and rapid detection technology. The main purpose of near infrared spectrum analysis is to extract the response of the physical and chemical information of different objects to the absorbance of near infrared light, and then to use the different responses of different objects and the physical and chemical information of the objects as a correlation mathematical model to realize the indirect analysis of the physical and chemical information of the objects by near infrared spectrum.
The near infrared spectrometer of the common laboratory generally comprises a light source 1', a monochromator 2', a detector 3', a sample measurement accessory and the like, the common structure is generally divided into an infrared spectrometer with front light splitting as shown in fig. 1, and the monochromator 2' is arranged in front of a sample 4 '; post-spectroscopic as in the infrared spectrometer of fig. 2, a monochromator 2 'is provided behind the sample 4'. The light source 1' emits light with continuous wavelength in near infrared region, which is dispersed into monochromatic light with each wavelength after passing through the monochromator 2', and then the monochromatic light irradiates the detector 3' to be converted into electric signal, and the electric signal is converted into digital signal by the circuit to obtain digital spectrum file composed of wavelength and absorbance. The monochromator is a spectroscopic device.
For infrared spectrometers, the main problem existing at present is that the spectrum data of sample detection is unstable, and the spectrum curves tested by each operation at different time are different, and the main reason is that the light source energy is too high to excite sample substances to generate fluorescence, raman light and the like, so that the detection result is affected. When the concentration of the sample is increased, the fluorescence generation efficiency is not increased in a linear relation, so that the fluorescence occupation ratio of the received spectrum is larger than that of the transreflective infrared spectrum, and the influence of fluorescence, raman light and the like on the detection result is further increased. According to the principle of fluorescence generation, fluorescence is generated by absorbing excitation light by molecules of a substance in a ground state in a normal state, and then changing the molecules in the excited state into an excited state, and the molecules in the excited state are unstable and release a part of energy in the form of light during the return to the ground state, thereby generating fluorescence. The emitted fluorescence wavelength is generally larger than the fluorescence excitation wavelength, so that the front-back single light-splitting structure of the existing infrared spectrometer cannot well eliminate fluorescence, raman light and other stray light possibly causing detection results.
Disclosure of Invention
The invention aims to solve the technical problems that: an optical system of an infrared spectrometer is designed to eliminate the influence of fluorescence, raman light and other stray light on an infrared spectrum detection result, and improve the repeatability and stability of the system.
In order to solve the problems, the invention adopts the following technical scheme: the utility model provides a dual-spectrum near infrared spectrometer based on supercontinuum laser, includes supercontinuum laser, leading beam splitting unit, post beam splitting unit and the detector that sets gradually according to the light path, leading beam splitting unit sets up before the sample, post beam splitting unit sets up behind the sample.
The front light splitting unit is a light dispersing device. The device is used for dispersing the red light continuous spectrum emitted by the supercontinuum laser into monochromatic light of each wavelength.
The rear light-splitting unit is a stray light filtering device. For filtering out stray light of non-infrared spectrum such as fluorescence generated by the sample and Raman light.
The front-end light splitting unit and the rear-end light splitting unit are one or more of a light filter type light splitting system, a grating scanning type light splitting system, a prism light splitting system, a Fourier transform type light splitting system, an acousto-optic tunable (AOTF) type light splitting system and a Hadamard variable type light splitting system.
The front light splitting unit and the rear light splitting unit are identical or different in structure.
The front light splitting unit and the rear light splitting unit have the same structure and comprise two toroidal reflectors and a grating, and light is reflected from one toroidal reflector to the grating and then to the other toroidal reflector. The toroidal mirror provides higher resolution and better beam quality.
The two toroidal reflectors and the grating adopt a symmetrical light path design or an asymmetrical light path design.
The optical properties of the two toroidal mirrors are the same or different.
A focusing reflector is arranged behind the supercontinuum laser. The focusing mirror is used to focus the light emitted by the laser.
The focusing mirror is a spherical mirror, an aspherical mirror or a free-form mirror.
The front light splitting unit or the rear light splitting unit is provided with a seam, and the rear light splitting unit or the front light splitting unit is provided with a seam.
When the sample is solid, the front light splitting unit and the rear light splitting unit are the same device.
The light is reflected to the sample through a spherical focusing mirror after passing through the front light-splitting unit, and the light reflected by the sample is reflected to the front light-splitting unit through the spherical focusing mirror.
When the sample is liquid, the front light splitting unit and the rear light splitting unit are two sets of equipment and are respectively arranged on two sides of the sample.
The rear parts of the front light splitting unit and the rear light splitting unit are respectively provided with a reflecting mirror.
The reflecting mirror is a reflecting mirror which makes the light path turn by 90 degrees.
The front beam splitting unit is provided with a free-form surface reflecting mirror, a tyre mirror or an off-axis ellipsoidal reflecting mirror, and the rear beam splitting unit is provided with a free-form surface reflecting mirror, a tyre mirror or an off-axis ellipsoidal reflecting mirror.
The grating of the front light splitting unit and the grating of the rear light splitting unit synchronously rotate.
The invention has the beneficial effects that:
the front light splitting unit and the rear light splitting unit are arranged in front of and behind the sample, so that the influence of stray light such as fluorescence, raman light and the like can be effectively filtered, the heat generated by the light source of the supercontinuum laser is small, and the repeatability and the stability of the instrument can be effectively improved; the light spot irradiated on the sample has stronger energy and smaller light spot, so that the sample fault analysis can be performed, and the using amount of the precious sample is saved.
Drawings
FIG. 1 is a schematic diagram of a front-end spectroscopic infrared spectrometer of the prior art;
FIG. 2 is a schematic diagram of a post-spectroscopic infrared spectrometer of the prior art;
FIG. 3 is a schematic diagram of a dual-spectroscopic near infrared spectrometer based on a supercontinuum laser according to the present invention;
fig. 4 is a schematic structural diagram of a front-end light splitting unit according to the present invention (the structure of a rear-end light splitting unit is the same as that of a front-end light splitting unit);
FIG. 5 is a schematic diagram of a dual-spectroscopic near infrared spectrometer based on a supercontinuum laser according to the first embodiment;
fig. 6 is a schematic structural diagram of a dual-spectroscopic near infrared spectrometer based on a supercontinuum laser according to the second embodiment.
Detailed Description
The structure and features of the present invention will be described in detail below with reference to the accompanying drawings and examples. It should be noted that various modifications can be made to the embodiments disclosed herein, and thus, the embodiments disclosed in the specification should not be taken as limiting the invention, but merely as exemplifications of embodiments, which are intended to make the features of the invention apparent.
The invention adopts the technical scheme that: the utility model provides a dual-spectrum near infrared spectrometer based on supercontinuum laser is as shown in fig. 3, includes supercontinuum laser light source 1, leading beam splitting unit 2, post beam splitting unit 3 and detector 4, leading beam splitting unit 2 sets up before sample 5, post beam splitting unit 3 sets up behind sample 5.
The front-end light splitting unit 2 and the rear-end light splitting unit 3 may be one or more of a filter-type light splitting system, a raster scanning-type light splitting system, a prism-type light splitting system, a fourier transform-type light splitting system, an acousto-optic tunable (AOTF) light splitting system, or a hadamard variable-type light splitting system. The front light splitting unit 2 and the rear light splitting unit 3 may have the same or different structures, so long as the purpose is achieved that the front light splitting unit 2 is a light dispersing device. The device is used for dispersing the red light continuous spectrum emitted by the supercontinuum laser into monochromatic light of each wavelength. The rear light-splitting unit 3 is a stray light filtering device for filtering stray light of non-infrared spectrum such as fluorescence and raman light generated by the sample.
More preferably, the front light splitting unit and the rear light splitting unit have the same structure and comprise a first toroidal mirror 10, a grating 11 and a first toroidal mirror 12, and light is reflected from one toroidal mirror to the grating 11 and then to the other toroidal mirror. The toroidal mirror provides higher resolution and better beam quality. The toroidal mirror 10 and the toroidal mirror 12 and the grating 11 may be of symmetrical or asymmetrical optical path design.
More preferably, the first toroidal mirror 10, the first toroidal mirror 12 and the grating 11 are symmetrical CT type coma-eliminating light path designs, as shown in FIG. 4. The optical performance of the two toroidal reflectors is the same or different and can be determined according to the design requirements of the system.
The back of the supercontinuum laser is provided with a reflecting mirror which can be a free-form surface reflecting mirror, a tyre mirror or an off-axis ellipsoidal reflecting mirror. A free-form mirror is preferred, with higher spot quality.
Whether the front light splitting unit 2 or the rear light splitting unit 3 is arranged, a seam is arranged at the front end, and a seam is arranged at the rear end.
Because the detection light paths of the solid sample and the liquid sample are different, according to the design principle of the double-beam-splitting near infrared spectrometer based on the supercontinuum laser, the structure is specifically described as follows:
embodiment one, a dual-spectral near infrared spectrometer for solid sample detection
As shown in fig. 5, according to the optical path, the dual-spectroscopic near infrared spectrometer for solid sample detection includes a supercontinuum laser 1, an aspherical mirror 6, a filter 7, an entrance slit 8, a spectroscope 9, a toroidal mirror 10, a grating 11, a toroidal mirror 12, an exit slit 13, an aspherical focusing mirror 14, a sample 5, an entrance slit 15, a focusing lens 16, and a detector 4. The spectroscope 9 is a perspective and reflection instrument.
The laser emitted by the supercontinuum laser 1 is focused by the aspheric mirror 6, filtered by the optical filter 7, passes through the entrance slit I8 and passes through the beam splitter 9 to reach the front beam splitting unit 2, namely, light irradiates on the toroidal mirror I10, reaches the grating 11 after being reflected, reaches the toroidal mirror II 12, the reflected light is reflected to the sample 5 by the aspheric focusing mirror 14 from the exit slit I13, the reflected light of the sample 5 again reaches the aspheric focusing mirror 14 to the entrance slit II 15, irradiates on the toroidal mirror II 12, then is reflected to the grating 11, reaches the toroidal mirror I10, and is reflected to the focusing lens 16 and the detector 4 by the beam splitter 9.
In order to save space, the first outlet slit 13 and the second inlet slit 15 are arranged as an integral structure, and the first outlet slit 13 and the second inlet slit 15 are different slits.
The arrows in the figure indicate the direction of the light path.
Embodiment two, double-spectroscopic near infrared spectrometer for liquid sample detection
As shown in fig. 6, according to the optical path, the dual-spectral near infrared spectrometer for solid sample detection includes a supercontinuum laser 1, an aspherical mirror 6, a filter 7, an entrance slit 8, a toroidal mirror 10, a grating 11, a toroidal mirror 12, an exit slit 13, a freeform mirror 14, a sample 5, a freeform mirror 15, an entrance slit 16, a toroidal mirror 17, a grating 18, a toroidal mirror 19, an exit slit 20, and a detector 4.
The laser emitted by the supercontinuum laser 1 is focused by the aspheric mirror 6, filtered by the optical filter 7, irradiated to the front beam splitting unit through the entrance slit I8, namely the toroidal mirror I10, irradiated to the toroidal mirror II 12 through the reflection grating I11, reflected light irradiates to the free-form surface mirror I14 through the exit slit I13, reflected to the sample 5, reflected to the free-form surface mirror II 15 through the sample 5, enters the entrance slit II 16, and reaches the rear beam splitting unit, namely the detector 4 through the exit slit II 20 after passing through the toroidal mirror III 17, the grating II 18 and the toroidal mirror IV 19.
The arrows in the figure indicate the direction of the light path.
The terms "front" and "rear" in the present invention are defined in terms of the direction of the optical path.
Advantages of new and existing infrared spectrometer systems
The super-continuum spectrum laser light source is adopted, so that the energy is stronger, the stability is higher, the heat generated by the light source is low, the problems of temperature drift and the like caused by temperature rise can be effectively solved, and the luminous quality of the laser light source is better;
the front light splitting unit and the rear light splitting unit of the double light splitting system are adopted, so that other stray light such as fluorescence and Raman light can be effectively restrained, and the repeatability and stability of the instrument are improved; the front light splitting unit and the rear light splitting unit of the liquid infrared spectrometer adopt a vertical double-layer structure, grating mechanisms of the front light splitting unit and the rear light splitting unit synchronously move, wavelength errors and the like caused by asynchronous grating rotation are reduced, and the solid infrared spectrometer adopts a front-rear integrated light splitting device structure;
the front light splitting unit and the rear light splitting unit adopt symmetrical CT type aberration eliminating systems, so that the resolution is higher, and the beam quality is better;
the focusing mirror adopts a free-form surface reflecting mirror, so that the energy of a light spot irradiated on a sample is stronger, and the area is smaller.
The invention provides a double-beam-splitting near infrared spectrometer based on a supercontinuum laser, which solves the problems in the prior art and can be used for detecting liquid and solid infrared spectrums.
The super-continuum spectrum laser light source comprises a super-continuum spectrum laser and a focusing reflector, wherein the focusing reflector adopts an aspheric reflector to improve the light spot quality;
the front light splitting system comprises a toroidal collimating mirror, a focusing mirror and a grating, and is connected with the light source part;
the external light path system comprises a free-form surface focusing reflecting mirror, a sample bin and a free-form surface receiving reflecting mirror, and is connected with the front-end light splitting unit;
the rear light splitting system comprises a toroidal collimating mirror, a focusing mirror and a grating, and is connected with the external light path system;
the detector is an InGaAs detector and is connected with the rear-mounted light splitting system;
the electric signal processing and collecting system is used for processing and collecting the electric signal output by the sample light receiving unit so as to obtain the light intensity of the sample light and calculate the transmissivity of the sample, and is connected with the sample light receiving unit through an optical path;
the control and data processing system is used for controlling the infrared light beam splitter to complete spectrum scanning, process data and display infrared transmission spectrum or absorption spectrum of the sample, and is connected with the electric signal processing and collecting system and the infrared light beam splitter.
The beam splitter system comprises a filter type monochromatic system, a grating scanning type monochromatic system, a prism beam splitting system, a Fourier transform type monochromatic system, an acousto-optic tunable (AOTF) type monochromatic system and a Hadamard variation type monochromatic system.
The invention has the beneficial effects that the front-end beam splitter and the rear-end beam splitter are arranged in front of and behind the sample, so that the influence of stray light such as fluorescence, raman light and the like can be effectively filtered, the heat generated by the light source of the super-continuum spectrum laser is small, and the repeatability and the stability of the instrument can be effectively improved; the light spot irradiated on the sample has stronger energy and smaller light spot, so that the sample fault analysis can be performed, and the using amount of the precious sample is saved.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the scope of the present invention should be included in the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (8)
1. The double-beam near infrared spectrometer based on the supercontinuum laser is characterized by comprising the supercontinuum laser, a front beam splitting unit, a rear beam splitting unit and a detector which are sequentially arranged according to an optical path, wherein the front beam splitting unit is arranged in front of a sample, the rear beam splitting unit is arranged behind the sample, the front beam splitting unit is a light dispersing device and is used for dispersing the continuous spectrum of red light emitted by the supercontinuum laser into monochromatic light with each wavelength, the rear beam splitting unit is a light filtering device, and the stray light is fluorescence and Raman light;
the front-end light-splitting unit is one or more of a light filter type light-splitting system, a grating scanning type light-splitting system, a prism light-splitting system, a Fourier transform type light-splitting system, an acousto-optic adjustable light-splitting unit and a Hadamard variable light-splitting unit; the rear-mounted light-splitting unit is one or more of a light-filtering type light-splitting unit, a raster scanning type light-splitting unit, a prism light-splitting system, a Fourier transform type light-splitting unit, an acousto-optic Adjustable (AOTF) type light-splitting unit and a Hadamard variable type light-splitting unit;
the front light splitting unit and the rear light splitting unit have the same or different structures;
the front light splitting unit and the rear light splitting unit have the same structure and comprise two toroidal reflectors and a grating, and light is reflected from one toroidal reflector to the grating and then to the other toroidal reflector;
when the sample is solid, the front light splitting unit and the rear light splitting unit are the same device;
when the sample is liquid, the front light splitting unit and the rear light splitting unit are two sets of equipment, and are respectively arranged on two sides of the sample, and the gratings of the front light splitting unit and the rear light splitting unit synchronously rotate.
2. The dual beam near infrared spectrometer of claim 1, wherein the two toroidal mirrors and the grating are configured with a symmetrical or asymmetrical optical path design.
3. The dual beam near infrared spectrometer of claim 1, wherein a focusing mirror is disposed behind the supercontinuum laser.
4. The dual beam near infrared spectrometer of claim 3, wherein the focusing mirror is a spherical mirror, an aspherical mirror, or a freeform mirror.
5. The dual-spectroscopic near infrared spectrometer according to claim 1, wherein an entrance slit is provided in front of the front spectroscopic unit or the rear spectroscopic unit, and an exit slit is provided behind the front spectroscopic unit or the rear spectroscopic unit.
6. The dual beam near infrared spectrometer of claim 1, wherein the light is reflected by a spherical focusing mirror onto the sample after passing through the front beam splitting unit, and wherein the light reflected by the sample is reflected by the spherical focusing mirror onto the front beam splitting unit.
7. The dual-spectroscopic near infrared spectrometer as claimed in claim 1, wherein the rear of the front spectroscopic unit and the rear spectroscopic unit are each provided with a reflecting mirror.
8. The dual beam near infrared spectrometer of claim 7, wherein a free-form surface mirror, a tire mirror or an off-axis ellipsoidal mirror is disposed behind the front beam splitting unit, and a free-form surface mirror, a tire mirror or an off-axis ellipsoidal mirror is disposed behind the rear beam splitting unit.
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