CN1101544C - Ultraviolet Raman spectrometer - Google Patents
Ultraviolet Raman spectrometer Download PDFInfo
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- CN1101544C CN1101544C CN 98113710 CN98113710A CN1101544C CN 1101544 C CN1101544 C CN 1101544C CN 98113710 CN98113710 CN 98113710 CN 98113710 A CN98113710 A CN 98113710A CN 1101544 C CN1101544 C CN 1101544C
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Abstract
The present invention relates to an ultraviolet Raman spectrometer which is mainly composed of a laser excitation light source, a light path system, a beam splitting system and a signal collecting and data processing system, and ultraviolet laser light with the wavelength of 200 to 400 nms is adopted as the excitation light source. The present invention can overcome the interference of surface fluorescence so that a Raman spectrum can exert potential functions in the research of catalyst surfaces.
Description
Technical field
The present invention relates to spectral analysis technique, a kind of ultraviolet Raman spectrometer is provided especially.
Background technology
Raman scattering is the inelastically scattered a kind of phenomenon of light and material, Raman spectrometer based on this phenomenon is modern important spectral analysis technique, in multiple subjects such as catalysis, surface, material and biological chemistry, have a wide range of applications, rely on it can obtain the important information of many related substance structures.In catalysis and Surface Science field, Raman spectrum can obtain the important information of material surface structure and surface species and structure and co-ordination state, especially can carry out the original position research of industrial catalyst and the quick and micro kinetics research of catalytic surface reaction.Traditional Raman spectrum many with visible or near-infrared laser as excitation source, its Raman signal just in time drops on phosphor region, so just be difficult to obtain Raman signal in case there is surface fluorescence to produce.How improving Raman spectrum, to make it give full play to its effect in catalytic surface research be a great problem for a long time always, Surface enhanced raman spectroscopy and near infrared FT-Raman spectrum once were used to overcome the interference of surface fluorescence, but failed fundamentally improving Raman spectrum.
In addition, visible Raman spectrometer has simply connected and two kinds of Application Design of multi-joint beam split at present in the spectra collection process: if adopt bigeminy or triplicate form look instrument, promptly be equivalent to two or three monochromator series connection, by repeatedly dividing light action, to reach maximum spectral resolution, this just makes detector can't carry out the detection of broad wave-number range, therefore more visible Raman spectrometer adopts the grating rotation to make light signal incide detector successively by wavelength and finishes spectra collection in the spectra collection process, and this cross the range request laser intensity remain constant, higher to the stability requirement of laser instrument and spectrometer; If only adopt the simply connected monochromator, how to filter strong Rayleigh signal, but because optics narrow band pass filter bandwidth is bigger, only (single monochromator parasitic light index generally can only reach 10 to background stray light through a monochromator elimination simultaneously with the optics narrow band pass filter
-4～10
-5), can only detect 200～300cm like this
-1Above Raman signal can not be surveyed the Raman signal of lower wave number scope.
(patent No.: CN1128063A) disclose a kind of off-axis optical system that is used for collecting and assembling electromagnetic radiation, it is that axle center shape is in an angle on the turning axle greater than zero degree that its Electromagnetic Launching source S and acceptance point T (impact point) drop on the elliptic geometry optic axis to Chinese patent.In addition, although the oval shape mirror of employing collection system is also arranged in the design in the past, but it need be combined by two optical mirror planes, the i.e. optical system that combines of the reflective mirror of ellipsoidal surface catoptron and wheel fetalism curved surface or sphere, can only be used on the general collection photosystem, the light of its collection generally can only directly obtain from some common light sources, the picture filament bulb, gas-discharge lamp, laser instrument, light emitting diode, semiconductor and optical fiber etc., the aberration and the astigmatism that produce in its light reflex process are wayward, and are difficult to use in the such instrument of Raman spectrum, and its needs bigger space and some adjustment racks just can carry out.
Summary of the invention
The object of the present invention is to provide a kind of ultraviolet Raman spectrometer, it can overcome the interference of surface fluorescence, the astigmatism of the aberration that is produced in the control reflection process is surveyed the information of lower wave number scope, thereby is made Raman spectrum bring into play the effect of its uniqueness in the research of catalyst surface.
The invention provides a kind of ultraviolet Raman spectrometer, mainly constitute by laser excitation light source, light path system, beam splitting system, signals collecting and data handling system four major parts, it is characterized in that: adopt wavelength at the Ultra-Violet Laser of 200～400nm as excitation source, the Raman spectrum that is used for liquid state, solid matter detects;
The scattered light of described light path system is collected the design that part adopts the ellipsoidal surface mirror, promptly intercept the part of ellipsoidal surface as the ellipsoidal surface mirror in the elliptical shaft direction, two focuses of ellipse respectively as the signal optical source of sample with collect the light focus point, the focal point F near the ellipsoidal surface mirror
1As the Raman emission light source point, described flashlight source point is positioned at outside the ellipsoidal surface mirror, another focal point F
2Collection light focus point as sample;
Described light path system concrete structure is: from the excitation source laser beam through first mirror M
8Light path is directed to second mirror M
9, second mirror M
9The minute surface setting make the laser and the ellipsoidal surface mirror optical axis that reflect overlapping, sample is placed on the signal optical source place, the scattered light that sample is subjected to produce behind the light source activation is as the Raman light signal source, the back-scattering light that sends from sample converges to collection light focus point through the ellipsoidal surface mirror, imports beam splitting system again;
Focal point F described ellipsoidal surface mirror, that the light focus point is collected in conduct
2The place ahead two convex lens that be arranged in parallel import beam splitting system with the light signal of collecting; Described converge at the ellipsoidal surface mirror, as the focal point F of collecting the light focus point
2Signal also can directly import beam splitting system;
Described beam splitting system be the parallel connection of first～bigeminy grating, again with the 3rd grating cascaded structure, wherein said first～bigeminy grating symmetry is installed, the complementation setting that grating surface indentation direction is opposite, the 3rd grating consists of the triangular structure setting by three blocks of gratings;
Described wavelength can be 228～229nm, 238～238.5nm, and 244.0nm, 257～257.5nm, medium ultraviolet optical maser wavelength is 325.0nm, near ultraviolet visible laser wavelength is 441.6nm;
In addition, the present invention can add visible light and near-infrared laser as excitation source; The visible laser wavelength can be 457.9,488.0,514.5nm.
Because Ultra-Violet Laser can make the fluorescence of catalyst surface stronger, thereby in research in the past, nobody proposes to adopt Ultra-Violet Laser to make the excitation source of Raman spectrum, to overcome the interference of surface fluorescence to Raman spectrum.In fact, after adopting Ultra-Violet Laser as excitation source, thereby Raman signal can move the fluorescence interference of having avoided the visible range to the ultraviolet region.After incident laser is transferred to the ultraviolet region from the visible range simultaneously, because shortened wavelengths also makes Raman scattering significantly strengthen.So the ultraviolet Raman not only can be avoided fluorescence interference but also sensitivity is increased substantially.Thereby obtain resonance Raman spectroscopy by regulating optical maser wavelength some molecular radical in can the selective excitation system, the present invention can high selectively obtain the structural information of a certain local part of molecule.These characteristics have clear superiority in the research of the big molecule of complexity, polymeric system, biomacromolecule.Simultaneously, the electronic of most of catalystic converter system drops on the ultraviolet region just, adopts Ultra-Violet Laser might excite the electronic state of system and produce resonance raman, makes Raman signal strengthen 10
2～10
6Thereby doubly further improve sensitivity.
In a word, the present invention has overcome technical prejudice and has 1. successfully avoided fluorescence interference, the helpless sample test of traditional Raman spectrum of making over becomes possibility, to tens kinds of up to a hundred various sample (solids, liquid) compare test, prove that the ultraviolet Raman can successfully avoid fluorescence interference; 2. sensitivity significantly improves, and for example, traditional Raman 100mw light source scan nearly one hour, and the ultraviolet Raman is only used the 5mw light source, and only scanning in tens seconds can obtain the spectral signal figure of same quality.Have following advantage in addition:
The scattered light of light path system is collected the design that part has adopted the ellipsoidal surface mirror among the present invention, promptly make the ellipsoidal surface catoptron in the part of elliptical shaft direction intercepting ellipsoidal surface, with two focuses of ellipse respectively as the excitation source of sample with collect the light focus point.By Electromagnetic Launching source (refer to launch after testing sample is via laser radiation Raman diffused light) and acceptance point are placed on the same elliptic geometry optic axis promptly so-called coaxial optical system.This kind design one confrontational collection light microscopic adopts the mode of diaphotoscope, and the one, solved the low problem of quartz glass ultraviolet transmission rate, also make the collection optical efficiency bring up to 35% on the other hand, thereby further improved the sensitivity of instrument by being no more than 10%; Again, oval shape mirror major axis first focus (promptly placing sample spot) is placed the ellipsoidal surface mirror outside that is cut, the collection rate and the operability of analytic sample signal have greatly been improved, aberration that is produced in its reflection process and astigmatism are controlled and are improved than the position that is easier to by the fine setting electromagnetic radiation source, are particularly suitable for being applied to the collection of spectrometer to feeble signal.
The position that sample of the present invention is placed is exactly the position in Electromagnetic Launching source, Electromagnetic Launching of the present invention source can be various gases, liquid or solid sample, when a branch of illumination is mapped on the sample, behind the certain energy of absorption of sample Raman diffused light takes place, another focus on the optic axis is collected this Raman diffused light and converge in the effect of oval cross section mirror exactly.And the position that sample is placed has been moved on to oval internal reflector outside, and this makes that the replacing sample is very convenient, and can assemble any other equipment on sample position, has opened up the range of application of this collection light microscopic greatly.
The present invention can install the catoptron of laser beam and not influence its luminous flux in oval minute surface reflexes to the light cone of oval second focal point F 2.The present invention successfully is applied to the improvement of Ultra-Violet Laser Raman spectrometer, has greatly improved the service efficiency of Raman spectrometer in conjunction with other inventions, makes to perplex traditional Raman spectral information collecting amount shortcoming little, that sensitivity is low for a long time and be improved.
Ultraviolet Raman spectrometer of the present invention can be widely used in catalysis, material, environmental protection and biological field.The use field of Raman spectrometer has greatly been expanded in the particularly application of laser Raman spectroscopy catalysis characterization technique in position aspect.
Description of drawings
Accompanying drawing 1 is the ultraviolet Raman spectrometer system layout.
Accompanying drawing 2 is the oval light path synoptic diagram of collecting in the light path system.
Accompanying drawing 3 is beam splitting system three grating monochromator index paths.
Accompanying drawing 4 is computer control and data acquisition system (DAS) sketch.
Accompanying drawing 5 is the in-situ Raman spectrum tool.
Accompanying drawing 6 be benzene visible light Raman spectrogram (457.9nm, 10s).
Accompanying drawing 8 be teflon visible light Raman spectrogram (457.9nm, 100s).
Accompanying drawing 9 be teflon ultraviolet light Raman spectrogram (257.25nm, 10s).
Accompanying drawing 10 be USY visible light Raman spectrogram (457.9nm, 100s).
Accompanying drawing 11 be USY ultraviolet light Raman spectrogram (244.0nm, 100s).
Embodiment
By embodiment in detail the present invention is described in detail below in conjunction with accompanying drawing.
Embodiment
As shown in Figure 1, ultraviolet Raman spectrometer is made of the Lights section, light path system, data acquisition and recording system three parts.
The Lights section has adopted the Inova 300 Fred ultraviolet lasers of three light source Coherent companies, the Ar+ ion laser of homemade He-Cd laser instrument and Spectra Physics company; The Inova300 Fred laser instrument of Coherent company can obtain several laser rays in the ultraviolet region; 257.2nm (100mW), 244.0nm (100mW), 228.9nm (10mW), and at 251.3nm, 248.2nm, 238.2nm also have considerable power output, homemade He-Cd laser instrument can obtain the power output of 20mW at 325nm; And the output of 5mW can have been satisfied the needs of uv raman spectroscopy.The Ar+ ion laser of Spectra-Physics company can obtain the laser output of watt level in the visible range.Thereby can from the ultraviolet to the visible light, (carry out resonance Raman Spectroscopic Study of Cytochrome in 200～600nm) wide regions.
Referring to accompanying drawing 2, described light path system (outer light path) concrete structure is: from the laser beam of laser through first mirror M
8Light path is directed to second mirror M
9, second mirror M
9The minute surface setting make the laser and the ellipsoidal surface mirror optical axis that reflect overlapping, to sample, sample is placed on the focal point F of ellipsoidal surface mirror along the laser radiation of ellipsoidal surface mirror optical axis
1The place and is positioned at outside the ellipsoidal surface mirror, and the back-scattering light that sends from sample is as the Raman light signal source, and optical signal source converges to another focal point F of ellipsoidal surface mirror through the ellipsoidal surface mirror
2, F
2As collecting the light focus point, present embodiment is in the focal point F of described ellipsoidal surface mirror
2The place ahead two convex lens that be arranged in parallel import beam splitting system with the light signal of collecting; In the described light path design, owing to used ellipsoidal surface mirror (all reaching 95% to the reflectivity in the 1200nm wavelength coverage) at 195nm, again because the ellipsoidal surface mirror had both played the collection mirror effect of light signal, also played the catoptron effect, played the condenser effect that light signal is assembled simultaneously, so in the Raman spectrum gatherer process, if replacing light source then whole optical path does not need to carry out any element replacement, instrumentation is very convenient, and designed ultraviolet Raman spectrometer also is applicable to the LASER Light Source from the visible range to the infrared region;
Referring to accompanying drawing 3, described beam splitting system adopts three grating monochromators, be specially the first bigeminy grating parallel connection, again with the 3rd grating cascaded structure, wherein said first～bigeminy grating symmetry is installed, the complementation setting that grating surface indentation direction is opposite, light path is from slit S
1To spatial filtering mirror M
3With light path from slit S
3To spatial filtering mirror M
3Be the optics symmetry, light signal is from slit S
1Incident is through grating G
1Back light signal is opened in spatial dispersion by wavelength, slit S
2After Rayleigh line cut out, through M
3Reflection.Because light path is a design symmetry, the light signal of chromatic dispersion is converged to S again
3, this moment S
3Light signal be equivalent to eliminate S behind the Rayleigh line
1The light signal at place; The 3rd grating consists of the triangular structure setting by three blocks of gratings, is mainly used in beam split, and its blaze of grating wavelength is in ultraviolet, visible and infrared band respectively, and it is maximum that the spectral response range of three blocks of gratings reaches in SPECTRAL REGION separately;
Beam splitting system of the present invention can be taken the photograph spectral limit at 185～1000nm, but front two grating G1, G2 filtering parasitic light and Rayleigh line, three grating G3, G4, G5 of the 3rd grating are used for beam split, and three gratings can be adjusted to be applicable to different LASER Light Source; The present invention has been owing to adopted this unique design of triplicate form look instrument that comprises symmetrical light path, has the background stray light of material impact can eliminate to very low that (its index is lower than 10 to raman spectroscopy measurement
-12～10
-15), and then this can detect and is low to moderate 20cm
-1Raman signal.
Signal collection has adopted highly sensitive ccd detector, can instantaneous acquired signal apace, and acquisition rate can reach Millisecond in theory, carries out data processing with the Pentium 133 computing machine, sees accompanying drawing 4.
Accompanying drawing 6～11 is respectively the visible light of benzene, teflon, VSY and the Raman spectrogram of ultraviolet light, and visible ultraviolet Raman has better resolution.Wherein: by accompanying drawing 8 as can be seen, because teflon has very strong fluorescence signal, and the Raman peaks intensity that is positioned on the fluorescence peak is compared very little with fluorescence signal.Thereby can only see several peaks that Raman peaks is more intense; By accompanying drawing 9 as can be seen, owing to avoided the hyperfluorescence signal of teflon, thereby can obtain teflon Raman peaks clearly, and detection time has only 1/10th of visible Raman spectrum; Referring to accompanying drawing 10,, survey less than Raman signal because the fluorescence of USY is stronger at all; Referring to accompanying drawing 11,, obtain USY Raman spectrogram clearly identical obtaining in the detection time.
The present invention can add visible light and near-infrared laser as excitation source, and its visible laser wavelength is 457.9,488.0,514.5nm.Of the present invention converge at the ellipsoidal surface mirror, as the focal point F of collecting the light focus point
2Signal also can directly import beam splitting system.
Claims (9)
1. ultraviolet Raman spectrometer, mainly constitute by laser excitation light source, light path system, beam splitting system, signals collecting and data handling system four major parts, it is characterized in that: adopt wavelength at the Ultra-Violet Laser of 200～400nm as excitation source, the Raman spectrum that is used for liquid state, solid matter detects.
2. by the described ultraviolet Raman spectrometer of claim 1, it is characterized in that: the scattered light of described light path system is collected the design that part adopts the ellipsoidal surface mirror, promptly intercept the part of ellipsoidal surface as the ellipsoidal surface mirror in the elliptical shaft direction, two focuses of ellipse respectively as the signal optical source of sample with collect the light focus point, the focal point F near the ellipsoidal surface mirror
1As the Raman emission light source point, described flashlight source point is positioned at outside the ellipsoidal surface mirror, another focal point F
2Collection light focus point as sample.
2. by the described ultraviolet Raman spectrometer of claim 1, it is characterized in that: described light path system concrete structure is: from the excitation source laser beam through first mirror M
8Light path is directed to second mirror M
9, second mirror M
9The minute surface setting make the laser and the ellipsoidal surface mirror optical axis that reflect overlapping, sample is placed on the signal optical source place, the scattered light that sample is subjected to produce behind the light source activation is as the Raman light signal source, the back-scattering light that sends from sample converges to collection light focus point through the ellipsoidal surface mirror, imports beam splitting system again.
3. by the described ultraviolet Raman spectrometer of claim 2, it is characterized in that: focal point F described ellipsoidal surface mirror, that the light focus point is collected in conduct
2The place ahead two convex lens that be arranged in parallel import beam splitting system with the light signal of collecting.
4. by the described ultraviolet Raman spectrometer of claim 2, it is characterized in that: described converge at the ellipsoidal surface mirror, as the focal point F of collecting the light focus point
2Signal also can directly import beam splitting system.
5. by the described ultraviolet Raman spectrometer of claim 1, it is characterized in that: described beam splitting system be the parallel connection of first～bigeminy grating, again with the 3rd grating cascaded structure, wherein said first～bigeminy grating symmetry is installed, the complementation setting that grating surface indentation direction is opposite, the 3rd grating consists of the triangular structure setting by three blocks of gratings.
6. by the described ultraviolet Raman spectrometer of claim 1, it is characterized in that: described wavelength can be 228～229nm, 238～238.5nm, and 244.0nm, 257～257.5nm, medium ultraviolet optical maser wavelength is 325.0nm, near ultraviolet visible laser wavelength is 441.6nm.
7. by claim 1,2 or 5 described ultraviolet Raman spectrometers, it is characterized in that: can add visible light and near-infrared laser as excitation source.
8. by the described ultraviolet Raman spectrometer of claim 7, it is characterized in that: the visible laser wavelength can be 457.9,488.0,514.5nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98113710 CN1101544C (en) | 1998-01-07 | 1998-01-07 | Ultraviolet Raman spectrometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98113710 CN1101544C (en) | 1998-01-07 | 1998-01-07 | Ultraviolet Raman spectrometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1222674A CN1222674A (en) | 1999-07-14 |
| CN1101544C true CN1101544C (en) | 2003-02-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 98113710 Expired - Lifetime CN1101544C (en) | 1998-01-07 | 1998-01-07 | Ultraviolet Raman spectrometer |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351624C (en) * | 2005-01-13 | 2007-11-28 | 上海众毅工业控制技术有限公司 | Dissolved gas analyzer of electric power transformer oil based on Raman technology |
| TWI472725B (en) * | 2014-01-17 | 2015-02-11 | Academia Sinica | Lens-chromatism spectrum measurement device and spectrum measurement method |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100405044C (en) * | 2005-01-05 | 2008-07-23 | 中国科学院长春光学精密机械与物理研究所 | Optical structure of vacuum ultraviolet and fluorescence spectrum instrument |
| CN101968381A (en) * | 2009-06-11 | 2011-02-09 | 必达泰克光电设备(上海)有限公司 | Raman spectroscopic apparatus and method for measuring raman spectrum containing fluorescent materials |
| DE102010044875A1 (en) * | 2010-09-09 | 2012-03-15 | Limo Patentverwaltung Gmbh & Co. Kg | Illumination device for producing a linear intensity distribution in a working plane |
| CN107449767A (en) * | 2016-06-01 | 2017-12-08 | 中国科学院大连化学物理研究所 | A kind of ultraviolet Raman fiber optic probe |
| CN106442565B (en) * | 2016-10-26 | 2019-06-21 | 中国科学院上海光学精密机械研究所 | The surface defect detection apparatus of high-rate laser line scanning |
| CN107505307B (en) * | 2017-08-09 | 2020-11-27 | 成都艾立本科技有限公司 | Full-surrounding type elliptical spherical mirror light path laser-induced breakdown spectrometer system |
-
1998
- 1998-01-07 CN CN 98113710 patent/CN1101544C/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351624C (en) * | 2005-01-13 | 2007-11-28 | 上海众毅工业控制技术有限公司 | Dissolved gas analyzer of electric power transformer oil based on Raman technology |
| TWI472725B (en) * | 2014-01-17 | 2015-02-11 | Academia Sinica | Lens-chromatism spectrum measurement device and spectrum measurement method |
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| Publication number | Publication date |
|---|---|
| CN1222674A (en) | 1999-07-14 |
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