CN101995387A - Multi-functional ultraviolet-visible spectrometer - Google Patents
Multi-functional ultraviolet-visible spectrometer Download PDFInfo
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- CN101995387A CN101995387A CN 201010281710 CN201010281710A CN101995387A CN 101995387 A CN101995387 A CN 101995387A CN 201010281710 CN201010281710 CN 201010281710 CN 201010281710 A CN201010281710 A CN 201010281710A CN 101995387 A CN101995387 A CN 101995387A
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Abstract
The invention discloses a multi-functional ultraviolet-visible spectrometer, which comprises an ultraviolet-visible light source, a fixed convex lens, an adjustable diaphragm, a movable convex lens, a turning apparatus, a charge coupled device (CCD) miniature spectrometer and a microcomputer. The multi-functional ultraviolet-visible spectrometer of the invention has a reflectance spectrum test function, a transmittance spectrum test function, an absorption spectrum test function, a scattered spectrum test function and a fluorescence spectrum test function, and can measure variations of the spectrum and the spectral intensity with angles through rotation of a sample table turning apparatus and a light-guide fibre turning apparatus, thereby obtaining a reflectance spectrum, a transmittance spectrum, a absorption spectrum, a scattered spectrum and a fluorescence spectrum which have angle resolution capability.
Description
Technical field
The present invention relates to a kind of spectral analysis testing apparatus, relate in particular to a kind of multi-functional ultraviolet-visible spectrometer.
Background technology
Transmitted spectrum, reflectance spectrum, absorption spectrum, scattering spectrum are the analytical test means of having many uses, and can be widely used in many fields, as material, physics, chemical, electronics, environment measuring, biological biochemistry, medicine etc.The structure of these spectrometers all is made up of a UV, visible light light source and beam split optical receiver basically, has a lot of something in commons on hardware.Yet these spectrometers exist with the form of simple function or difunctional spectrometer mostly at present.For example, do not considering under the reflection prerequisite of sample surfaces that transmitted light spectrometer (T) and absorption spectrometer (A) often are integrated in the spectrometer, promptly obtain absorption spectrum by A=1-T from transmitted spectrum.Generally speaking, because the value of reflectance spectrum (R) is less and do not have line structure, therefore absorption spectrum and the actual conditions that obtain like this are more or less the same.If but the reflection of sample is very strong, for example high index of refraction sample, or sample is the film sample of surfacing, and then the reflection of sample surfaces can not be ignored, the absorption spectrum that is obtained by 1-T just has bigger error so, and at this moment absorption spectrum should be A=1-T-R.For some sample,, so also must consider the influence of scattered light S because sample surfaces is more coarse.Scattering spectra S not only can further revise the value of absorption spectrum, and can obtain the information of the aspects such as size, surfaceness such as particle the sample from scattering of light spectrum.Though present commercial spectrometers can obtain reflectance spectrum by increasing means such as reflection annex or integrating sphere, but the reflectance spectrum with angle-resolved function that the present invention proposes has but comprised more information, because contain the relevant information of a lot of material behaviors in the reflectance spectrum with the angle variation.On the other hand, fluorescence spectrophotometer also is a kind of important analytical test means, but owing to need monochromatic light to excite and a photon detector that sensitivity is higher, therefore commercial fluorescence spectrophotometer not with transmission (absorption) spectrometer to combining, but independently be a testing apparatus.See on the cost of slave unit so not only uneconomically, see also from the instrument and equipment occupation space and to calculate that the information that obtains from the spectrometer of simple function when prior is often not comprehensive.The present invention makes full use of characteristics and the fibre-optic flexibility that CCD micro spectrometer data collection rate is fast, dynamic range is big, highly sensitive, has designed a kind of multi-functional ultraviolet-visual spectrometer that can finish transmission, reflection, scattering, absorption, fluorescence spectral measuring on same spectrometer.So not only the total cost of lowering apparatus equipment greatly also can reduce taking up room of instrument and equipment, improves test speed, more importantly is to have considered that the absorption spectra data that obtains after the reflection is more accurately reliable.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of multi-functional ultraviolet-visible spectrometer is provided.
The objective of the invention is to be achieved through the following technical solutions: a kind of multi-functional ultraviolet-visible spectrometer, it comprises: ultraviolet-visible light source, fixedly convex lens, adjustable diaphragm, removable convex lens, corner instrument, CCD micro spectrometer and microcomputer.Wherein, before ultraviolet-visible light source, convex lens, adjustable diaphragm and removable convex lens were sequentially arranged in the corner instrument, the corner instrument comprised sample stage, sample stage front and back regulating device, sample stage gyrator, optical fiber gyrator and fibre-optical fixator; Sample stage is fixed on the sample stage gyrator by regulating device before and after the sample stage, fibre-optical fixator is fixed on the optical fiber gyrator, fibre-optical fixator links to each other with the CCD micro spectrometer by ultraviolet-visible photoconduction fiber, and the CCD micro spectrometer links to each other with microcomputer by USB cable.
Further, comprise that also the fixedly convex lens support and of support fixation convex lens supports the removable convex lens support of removable convex lens.
Further, also comprise a pluggable bandpass filter and bandpass filter support, bandpass filter places between adjustable diaphragm and the removable convex lens, and bandpass filter is by the bandpass filter stent support.
The invention has the beneficial effects as follows that the multi-functional ultraviolet-visible spectrometer of the present invention has reflection (R), transmission (T), absorption (A), scattering (S), fluorescence spectrum (F) test 5 big functions.By the rotation of sample stage gyrator and light transmitting fiber gyrator, can measure the variation of above-mentioned spectrum and above-mentioned spectral intensity respectively with angle, obtain reflection, transmission, absorption, scattering, fluorescence spectrum thus with angular resolution.
When measuring transmitted spectrum, regulate sample stage gyrator A and optical fiber gyrator B, make α＞0, β=-α, i.e. sample stage gyrator angle A=α, optical fiber gyrator angle B=0 degree.This moment, incident ray was gone into the optical fiber inlet through the sample transmission is laggard.
When measuring reflectance spectrum, rotate sample stage gyrator A and optical fiber gyrator B, make α=β, i.e. sample stage gyrator angle A=α, optical fiber gyrator angle B=2 α, this moment, emergent ray was in the reflection direction of incident ray.
During absorbance spectrum, under the condition of sample stage gyrator angle A=α and optical fiber gyrator angle B=0 degree, measure transmitted spectrum T earlier, keep A=α constant then, rotate optical fiber gyrator B and make β=α, be B=2 α, measure the reflectance spectrum R of this moment, calculate by A=1-T-R again and obtain absorption spectrum.
When measuring scattering spectrum, rotate the sample stage gyrator and make A=α=90 spend, promptly incident light impinges perpendicularly on the sample surfaces.Rotation optical fiber gyrator makes can measure the scattering spectrum under the different emergence angle β by B=90+ β.
When measuring fluorescence spectrum, need on filter holder, to insert the bandpass filter of the required excitation wavelength correspondence of a slice to obtain the required monochromatic light of fluorescence excitation.Rotate sample stage gyrator and optical fiber gyrator, make α ≠ β, promptly B ≠ 2 α directly enter the mouth by reflecting into into optical fiber to avoid excitation source.
Description of drawings
Fig. 1 is multi-functional ultraviolet-visible spectrometer structural representation;
Fig. 2 is the transmitted spectrum of mocvd method Grown GaN film on the sapphire substrate;
Fig. 3 is the reflectance spectrum of mocvd method Grown GaN film on the sapphire substrate;
Fig. 4 is the absorption spectrum of mocvd method Grown GaN film on the sapphire substrate;
Fig. 5 is the scattering spectra on sintering ZnO ceramics sample surface;
Fig. 6 is the fluorescence emission spectrum of Mn:Zn2SiO4 ceramics sample;
Among the figure, ultraviolet-visible light source 1, fixedly convex lens 2, fixedly regulating device 10, sample stage gyrator 11, optical fiber gyrator 12, fibre-optical fixator 13, ultraviolet-visible photoconduction fiber 14, CCD micro spectrometer 15, USB cable 16, microcomputer 17 before and after the convex lens support 3, adjustable diaphragm 4, bandpass filter support 5, pluggable bandpass filter 6, removable convex lens support 7, removable convex lens 8, sample stage 9, sample stage.
Embodiment
The multi-functional ultraviolet-visual spectrometer of the present invention comprises: ultraviolet-visible light source 1, fixedly convex lens 2, adjustable diaphragm 4, removable convex lens 8, corner instrument, CCD micro spectrometer 15 and microcomputer 17.
Wherein, before ultraviolet-visible light source 1, convex lens 2, adjustable diaphragm 4 and removable convex lens 8 were sequentially arranged in the corner instrument, the corner instrument comprised sample stage 9, sample stage front and back regulating device 10, sample stage gyrator 11, optical fiber gyrator 12 and fibre-optical fixator 13; Sample stage 9 is fixed on the sample stage gyrator 11 by regulating device 10 before and after the sample stage, fibre-optical fixator 13 is fixed on the optical fiber gyrator 12, fibre-optical fixator 13 links to each other with CCD micro spectrometer 15 by ultraviolet-visible photoconduction fiber 14, and CCD micro spectrometer 15 links to each other with microcomputer 17 by USB cable 16.
The present invention comprises that also the fixedly convex lens support 3 and of support fixation convex lens 2 supports the removable convex lens support 7 of removable convex lens 8.
The light warp that ultraviolet-visible light source 1 sends fixedly convex lens 2 becomes directional light, incide on the sample of sample stage 9 through adjustable diaphragm 4 and removable convex lens 8 after, the reflected light of sample, scattered light, transmitted light import CCD micro spectrometer 15 into through ultraviolet-visible photoconduction fiber 14, CCD micro spectrometer 15 is spectroscopic data with the phototransformation that receives and is transferred on the microcomputer 17 by USB cable 16, reflects, scattering, transmission and absorption spectroanalysis.
The present invention also comprises a pluggable bandpass filter 6, bandpass filter 6 places between adjustable diaphragm 4 and the removable convex lens 8, bandpass filter 6 supports by bandpass filter support 5, like this, the light warp that ultraviolet-visible light source 1 sends fixedly convex lens 2 becomes directional light, through after the adjustable diaphragm 4, become monochromatic light by bandpass filter 6, shine on the sample of sample stage 9, make sample produce fluorescence, carry out fluorescent spectroscopy through CCD micro spectrometer 15 and microcomputer 17.
Ultraviolet-visible light source 1 provides measures required ultraviolet-visible light source, fixedly become flat pattern light behind the diverging light planoconvex lens that convex lens 2 make light source 1 send, adjustable diaphragm 4 is used to control the diameter of incident light intensity and parallel beam, measure for transmission, reflection, absorption and scattering spectrum, the diameter of limit light aperture should not be excessive to obtain less beam spot diameter, and higher angular resolution, and for fluorescence spectral measuring, the diameter of limit light aperture can suitably increase so that the fluorescence signal that sample produces is stronger.Pluggable bandpass filter is used for fluorescence spectral measuring, and it makes incident light become the required monochromatic light of fluorescence spectral measuring and produces fluorescence with excited sample.Removable convex lens 8 are used for fluorescence spectral measuring, and purpose is to make directional light assemble on sample 9 to strengthen the light intensity of incident light, finally makes sample produce stronger fluorescence signal.
In sum, the present invention proposes a kind of multifunctional light spectrometer that integrates transmitted spectrum, reflectance spectrum, absorption spectrum, scattering spectrum and fluorescence spectrum.By the combination of sample stage gyrator and optical fiber gyrator angle and the cooperation of bandpass filter and convex lens, can realize above-mentioned various spectrum function.
In following examples, used light source is the UV, visible light light source of the deuterium lamp combination of the iodine-tungsten lamp of a 50W and 20W, and the CCD spectrometer adopts the HR4000 type CCD spectrometer of U.S. marine optics company, and light transmitting fiber is a ultraviolet-visible photoconduction fiber.Carry out selecting for use the allusion quotation tungsten lamp as light source when transmitted spectrum, reflectance spectrum, absorption spectrum and scattering spectrum are measured; When carrying out fluorescence spectral measuring, select for use deuterium lamp as excitation source, and insertion a slice centre wavelength is the required excitation wavelength of bandpass filter acquisition of 254nm in filter holder, in order to improve launching efficiency, move into light path to movable convex lens this moment, make incident light be focused at sample surfaces, improve fluorescence intensity with this.
Before measuring, sample stage, sample stage gyrator angle and optical fiber gyrator angle that must pair spectrometer position and proofread and correct.Step is as follows:
(1) open the allusion quotation tungsten lamp, the diameter of selection limit light aperture such as 0.5mm do not place any sample to obtain less spot diameter on the sample stage.The optical fiber inlet is forwarded on the direction relative with incident ray, carefully regulate the optical fiber gyrator, make that line strength maximum that the CCD spectrometer is collected, the optical fiber gyrator angle B that sets this moment are 0 degree.
(2) put into sample this moment, the angle of carefully regulating the sample stage gyrator makes the signal maximum that the CCD spectrometer is collected, and guarantees that incident light skims over sample surfaces.
(3) move forward and backward sample stage, the signal intensity that makes the CCD spectrometer receive is about 1/2 when not placing sample.
(4) can set the angle A of sample stage gyrator this moment is 0 degree, and locking sample stage mobile device.
Instrumental correction finishes.
Describe the present invention in detail according to embodiment below, it is more obvious that purpose of the present invention and effect will become.
Embodiment 1: transmitted spectrum
Fig. 2 is the transmission spectrum T that utilizes mocvd method Grown GaN film on Sapphire Substrate, angle A=the α of sample stage gyrator during measurement=45 degree, optical fiber gyrator angle B=0 degree, normal incidence was in optical fiber after promptly incident light saw through sample, and the diameter of limit light aperture is 0.5mm.From the visible intensity in transmission vibration that significantly causes of Fig. 2 owing to the GaN thin film interference effects.Because the data of CCD spectrometer synchronous collection all wavelengths, it is very fast therefore to collect data, and the full spectra measurement time is 0.1 second only.
Embodiment 2: reflectance spectrum
Adopt the sample identical, and keep other experiment parameters constant, only change optical fiber gyrator angle B and cause β=45 degree with embodiment 1, i.e. B=alpha+beta=45+45=90 degree, optical fiber entered the mouth and was positioned on the reflection direction of incident beam this moment.The reflectance spectrum R that measures as shown in Figure 3.As seen also have in the reflectance spectrum significantly because the reflection strength that the GaN thin film interference effects causes vibration.Careful observation as seen, the maximum value in the transmitted spectrum is just in time corresponding to the minimal value in the reflectance spectrum.Equally, also minimum big corresponding in the reflectance spectrum just in time of the minimal value in the transmitted spectrum.
Embodiment 3: absorption spectrum
General ultraviolet-can be with spectrometer from the transmitted spectrum T spectrum A that is absorbed, has been ignored the influence of the oscillation of intensity that sample surfaces reflection R and film interference cause by A=1-T formula conversion.In the multifunctional light spectrometer of our invention,, can measure reflectance spectrum again, so conversion formula becomes A=1-T-R owing to both can measure transmitted spectrum.Utilize the principle of the oscillation of intensity complementation that interference causes in transmission spectrum and the reflectance spectrum intensity, can eliminate to a great extent owing to interfere the oscillation of intensity that causes.The absorption spectrum A=1-T-R that Fig. 4 obtains for the data by transmission spectrum T shown in Figure 2 and reflectance spectrum R shown in Figure 3.For the purpose of comparison, give the absorption spectra of utilizing conventional method A=1-T to provide among the figure.As seen, after considering the influence of film surface reflection R, oscillation of intensity among oscillation of intensity among the transmitted spectrum T and the reflectance spectrum R is just in time cancelled each other, therefore the oscillation of intensity among the absorption spectrum A=1-T-R is very little, the absorption edge that records thus is more near the energy gap of GaN film, and have tangible oscillation of intensity phenomenon among the absorption spectrum A=1-T-R that obtains when considering the influencing of reflection, not only located absorption value at the wavelength (photon energy) that absorption should not be arranged, and because the influence of oscillation of intensity causes absorption edge energy (being equivalent to energy gap) obviously less than normal.Attention compares for the energy gap with the GaN film, and the horizontal ordinate among Fig. 4 is photon energy hv.
Embodiment 4: scattering spectrum
Fig. 5 is several scattered light spectrograms of collecting from the ZnO ceramic surface of high temperature sintering.Sample stage gyrator angle A=α is 90 degree during test, and the diameter of limit light aperture is 0.5mm, and scattering angle β is respectively 15 degree, 30 degree, and 60 degree, promptly optical fiber gyrator angle B is respectively 105 degree, 120 degree, 150 degree.As seen not only relevant from the light intensity of sample surfaces scattering, and relevant with scattering angle β with wavelength.Further analysis can obtain the information of sample surface flatness or film endoparticle size.Since scattered light intensity relatively a little less than, the full spectra measurement time was increased to for 5 seconds.
Embodiment 5: fluorescence spectrum
Select for use deuterium lamp as excitation source during fluorescence spectral measuring.Because fluorescence signal intensity is very weak, therefore selecting the diameter of limit light aperture for use is 2.0cm, move into movable convex lens and make incident ray focus on sample surfaces, the CCD spectrometer adopts the mode that adds up for a long time to collect data (60 seconds) to obtain higher signal to noise ratio (S/N ratio) simultaneously.Fig. 6 is from mixing the fluorescence spectrum figure that Mn zinc silicate ceramics sample is collected.Sample stage gyrator angle A=α is 0 degree during test, optical fiber gyrator angle B=alpha+beta=45 degree, and optical filter is that centre wavelength is the bandpass filter of 254nm, diameter 2.54cm.
Claims (3)
1. multi-functional ultraviolet-visible spectrometer, it is characterized in that it comprises: ultraviolet-visible light source (1), fixedly convex lens (2), adjustable diaphragm (4), removable convex lens (8), corner instrument, CCD micro spectrometer (15) and microcomputer (17).Wherein, ultraviolet-visible light source (1), before fixedly convex lens (2), adjustable diaphragm (4) and removable convex lens (8) are sequentially arranged in the corner instrument, the corner instrument comprises regulating device (10) before and after sample stage (9), the sample stage, sample stage gyrator (11), optical fiber gyrator (12) and fibre-optical fixator (13); Sample stage (9) is fixed on the sample stage gyrator (11) by regulating device (10) before and after the sample stage, fibre-optical fixator (13) is fixed on the optical fiber gyrator (12), fibre-optical fixator (13) links to each other with CCD micro spectrometer (15) by ultraviolet-visible photoconduction fiber (14), and CCD micro spectrometer (15) links to each other with microcomputer (17) by USB cable (16).
2. according to the described multi-functional ultraviolet-visible spectrometer of claim 1: it is characterized in that, can also comprise that the fixedly convex lens support (3) and of support fixation convex lens (2) supports the removable convex lens support (7) of removable convex lens (8).
3. according to the described multi-functional ultraviolet-visible spectrometer of claim 1: it is characterized in that, can also comprise a pluggable bandpass filter (6) and bandpass filter support (5), bandpass filter (6) places between adjustable diaphragm (4) and the removable convex lens (8), and bandpass filter (6) supports by bandpass filter support (5).
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| CN103528684A (en) * | 2012-10-10 | 2014-01-22 | 中国科学院理化技术研究所 | Micro-area variable-angle spectrum test system |
| CN103776534A (en) * | 2014-03-05 | 2014-05-07 | 哈尔滨工业大学（威海） | Area array charge coupled device (CCD) prism spectrograph and space-time accumulation data processing method thereof |
| CN104296873A (en) * | 2014-10-10 | 2015-01-21 | 核工业北京地质研究院 | Spectrum bi-direction measuring system |
| CN106483093A (en) * | 2016-11-16 | 2017-03-08 | 江苏智石科技有限公司 | A kind of Content of Soil Component detection means based on rotation |
| CN110160651A (en) * | 2019-04-02 | 2019-08-23 | 四川双利合谱科技有限公司 | A kind of fluorescent high spectrum testing system |
| CN110487686A (en) * | 2019-09-03 | 2019-11-22 | 中国工程物理研究院流体物理研究所 | A kind of multi-modal spectroscopic diagnostics device of air conjugate heat transfer methodology and diagnostic method |
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| CN103528684A (en) * | 2012-10-10 | 2014-01-22 | 中国科学院理化技术研究所 | Micro-area variable-angle spectrum test system |
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| CN103776534A (en) * | 2014-03-05 | 2014-05-07 | 哈尔滨工业大学（威海） | Area array charge coupled device (CCD) prism spectrograph and space-time accumulation data processing method thereof |
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| CN104296873A (en) * | 2014-10-10 | 2015-01-21 | 核工业北京地质研究院 | Spectrum bi-direction measuring system |
| CN106483093A (en) * | 2016-11-16 | 2017-03-08 | 江苏智石科技有限公司 | A kind of Content of Soil Component detection means based on rotation |
| CN110160651A (en) * | 2019-04-02 | 2019-08-23 | 四川双利合谱科技有限公司 | A kind of fluorescent high spectrum testing system |
| CN110160651B (en) * | 2019-04-02 | 2022-03-08 | 江苏双利合谱科技有限公司 | Fluorescence hyperspectral testing system |
| CN110487686A (en) * | 2019-09-03 | 2019-11-22 | 中国工程物理研究院流体物理研究所 | A kind of multi-modal spectroscopic diagnostics device of air conjugate heat transfer methodology and diagnostic method |
| CN113567483A (en) * | 2020-08-31 | 2021-10-29 | 中国科学院上海硅酸盐研究所 | Multi-scale heterogeneous porcelain glaze nondestructive testing method based on element distribution and color spectrum combination |
| CN114486881A (en) * | 2021-12-27 | 2022-05-13 | 深圳市利拓光电有限公司 | Photonic crystal laser, light condensation adjusting method and gas detection device |
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