CN104931479A - Integrated imageable portable laser-Raman spectrum detector - Google Patents
Integrated imageable portable laser-Raman spectrum detector Download PDFInfo
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- CN104931479A CN104931479A CN201510334471.0A CN201510334471A CN104931479A CN 104931479 A CN104931479 A CN 104931479A CN 201510334471 A CN201510334471 A CN 201510334471A CN 104931479 A CN104931479 A CN 104931479A
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Abstract
The invention discloses a portable analytical instrument with the high integration degree and an imaging function based on the laser-Raman spectrum technology, and belongs to the technical field of portable analytical instruments. An integrated imageable portable laser-Raman spectrum detector is composed of a laser tube, a mechanical displacement module, a motor and power source power supply module, an integrated optical circuit module and a high-sensitivity micro spectrograph. The laser tube, the mechanical displacement module, the motor and power source power supply module, the integrated optical circuit module and the high-sensitivity micro spectrograph are installed in an instrument frame together in an integrated mode. Integrated design is adopted in a microimaging optical circuit and a Raman spectrum collecting optical circuit, the precise position of a laser spot on the surface of a sample is imaged to a CCD image sensor in real time, and therefore positioning analysis on the sample is achieved. The design that a high-sensitivity optical circuit system carries a small motor to drive a precision displacement table is adopted, compact circuit configuration is matched with the small high-sensitivity spectrograph, the whole size of the spectrograph is reduced to a micro size, and operation is facilitated. The overall micro design and the overall size and weight of the instrument are heavily optimized, and miniaturization and portability are achieved.
Description
Technical field
The invention belongs to portable analysers technical field, be specifically related to a kind ofly adopt the portable analysers that the integrated level of laser Raman spectroscopy technology is high, have imaging function.
Background technology
Portable analysis instrument: traditional test in laboratory means and main equipment, by the conjunctive use of the detection means of the industrial design of Highgrade integration, supersensitive checkout equipment and high stability, are transformed into portable and are easy to the microminiaturized analyser that operates by portable analysis instrument.It has that stability is high, fast response time, convenient operation, be easy to carry about with one, the feature such as strong adaptability.Portable analysis instrument has a wide range of applications in fields such as engineer operation monitoring, safety inspection, jewel explorations.
Laser Raman spectroscopy: laser Raman spectroscopy provides the information in the molecule aspect of material, at qualification material composition, defines on inner molecular structure, has great application.Laser Raman spectroscopy has multinomial technical characterstic: (1) laser raman is a kind of high information quantity analysis means exempting to mark, can realize component analysis; (2) be easy to multinomial technical method combine, can arrange in pairs or groups other detection means of laser Raman spectroscopy carries out more careful quantitative test, as atomic force microscope, mass spectrum etc.Laser Raman spectroscopy mating surface strengthens Raman scattering techniques (SERS), even can realize the detection of single molecules level, make it to be widely used as the supersensitive detection means of one.
The analytical approach that portable analysis instrument on market adopts is diversified trend.The sensing detection means that common hand-held analyzer is applied have a lot, such as semiconductor sensing, electric chemical formula sensing, catalytic combustion type sensing, photoionization formula sensing, spectrum sensing etc.The spectrum sensing means of common portable analysis instrument application have X-ray fluorescence spectra, infrared spectrum, fluorescence spectrum, Raman spectrum etc.Commercial Portable Raman optical spectrum analyser develops rapidly in the international market, the IDRaman mini spectrometer series of such as U.S. ocean company of company, and the NanoRam spectrometer series of BWTEK company.The Raman spectrometer of miniaturization is still combined with fibre-optical probe by the design concept of its Portable Raman optical spectrum analyser, can not be called the analytical instrument of integration.
For imageable Portable Raman optical spectrum detector, need to realize following requirement:
1. micro-imaging light path and Raman spectrum excite, gather light path integrated design, reduce the machine error impact that numerous device brings.
2. integrated modular design.Ensure instrumental function realize, highly sensitive while, the design of integrated modular improves the stability of instrument self, improve optical instrument itself strict demand measure of precision.
Summary of the invention
The object of this invention is to provide and a kind ofly adopt the portable analysers (typical sizes of instrument described in embodiment is: long 28cm, wide 7cm, high 19cm) that the integrated level of laser Raman spectroscopy technology is high, have imaging function.It is made up of the laser tube be arranged in apparatus frame (3), mechanical shift module, motor and light source power supply module (7), integrated optical circuit module (8) (comprise the imaging optical path that carries high resolution CCD and Raman signal excites and collects light path) and high-sensitivity miniature spectrometer (5) five part, with object lens in integrated optical circuit module (8) straight up direction be that instrument normally uses putting position.
Mechanical shift module is by a DC micromotor (6) and a fine bits moving stage (SIGMA KOKI company's T SDS-651S-M6 fine bits moving stage, displacement range 13mm) (2) composition, DC micromotor (6) is vertically fixed on the side of fine bits moving stage (2), and integrated optical circuit module (8) is fixed in fine bits moving stage (2).DC micromotor (6) when rotated, it is moving up and down of 10mm that top telescopic mast can do scope, under the drive of DC micromotor (6), fine bits moving stage (2) can be implemented in the fine bits transposition joint within the scope of vertical direction 10mm, thus realizes the focusing of the middle object lens of integrated optical circuit module (8) at sample surfaces.
Wherein, laser tube (3) and micro fiber spectrometer (5), can use the integral time etc. of the output power of unified control software design control laser tube, lighting time, spectrometer.
Integrated optical circuit module is by using a slice dichroic beamsplitter (Semrock company of the U.S., model FF776-Di01, working range: R>98%450 ~ 764nm, T>88%>789nm, wherein R represents reflectivity, T represents transmissivity) micro-imaging light path, laser Raman spectroscopy are excited and gathers light path and integrate, and be mounted on fine bits moving stage and enable along with fine bits moving stage does movement of focusing down on the whole, form the laser Raman spectrometer that integrated level is high, possess imaging function.
Wherein laser Raman spectroscopy excite with gather laser tube that optical routing wavelength is 785nm (being placed in apparatus frame), extender lens group, bandpass filter, dichroic beamsplitter, focus lens group, object lens and near infrared spectrometer form.Its course of work is as follows: by laser tube (3, Fuzhou of China Photop Technologies companies, model: PT20202) laser that sends is by being delivered in light path module (8) by fiber coupler (23) by laser again after Optical Fiber Transmission, expand through extender lens group (15) or become directional light in the horizontal direction, parasitic light is filtered again through bandpass filter (T>90%780 ~ 790nm) (16), then with the incident angles of 45 degree to 785nm double-tone spectroscope (R>98%785nm, T>90%841 ~ 1600nm) on (17), reflected light is vertically from bottom to top through dichroic beamsplitter (R>98%450 ~ 764nm, T>88%>789nm) (12) transmission, sample (30) is irradiated on the surface through detection window (4) after being focused on by object lens (10) again, sample (30) surface excites the Raman signal of lower generation to collect via object lens (10) at incident light, vertically from the top down successively through dichroic beamsplitter (R>98%450 ~ 764nm, T>88%>789nm) (12), 785nm double-tone spectroscope (R>98%785nm, T>90%841 ~ 1600nm) (17), again through the long pass filter of 785nm (semrock company of the U.S., model: BLP01-785R-25x36, T>90%>812.1nm) (18) filter Rayleigh scattering light, expand through flashlight shaping lens (19) or become directional light, after Raman signal fiber coupler (22), by optical fiber, Raman signal is transported to micro spectrometer (5, Fuzhou of China Photop Technologies companies, model: PT20007) in carry out data analysis and process.
Wherein micro-imaging optical routing LED white light source, focus lens group, a slice half-reflecting half mirror (R=50%350-750nm, T=50%350 ~ 750nm), a slice dichroic beamsplitter, object lens and CCD (Sony company 960H CCD Sensor, resolution: 720*576) imageing sensor form.Its course of work is as follows: by LED white light source (21) outgoing white light vertically from bottom to top planoconvex lens (20) assemble after with the incident angles of 45 degree on half-reflecting half mirror (11), through half-reflecting half mirror (11) reflection after in the horizontal direction with the incident angles of 45 degree to dichroic beamsplitter (R>98%450 ~ 764nm, T>88%>789nm) on (12), be irradiated to through detection window (4) after reflected light is vertically focused on by object lens (10) more from bottom to top and be positioned at sample (30) on object lens (10) back focal plane on the surface, the reflected light on sample (30) surface vertically becomes directional light from the top down after object lens (10), then with the incident angles of 45 degree to dichroic beamsplitter (R>98%450 ~ 764nm, T>88%>789nm) on (12), reflected light is in the horizontal direction through half-reflecting half mirror (11), focus on convex lens (13) focal imaging on CCD (14), make laser facula at the exact position real time imagery of sample surfaces to ccd image sensor, thus realize the positioning analysis of sample.
Innovation involved in the present invention and advantage:
(1) the present invention is by dichroic beamsplitter (R>98%450 ~ 764nm, traditional micro-imaging light path and spectra collection light path are be distributed into by dichroic beamsplitter the function modoularization project organization that picture and spectrogram gather spectral band by the mechanical type switching-over light path Integration Design of drag link mechanism toggle reflections prism by use T>88%>789nm).As above design provides two place's advantages: (a) decreases the volumetric spaces that double light path takies; B each device fixed placement in () light path system, the machine error that the mechanically actuated avoiding light path switching brings, improves spatial stability.This two places advantage applies, when the framework of the different detected sample system of Instrument Matching, can ensure reliability and the accuracy of analyzing data.
(2) the present invention adopts micro-imaging light path and Raman spectrum to gather light path part integrated design, can make laser facula at the exact position real time imagery of sample surfaces to ccd image sensor, thus realize the positioning analysis of sample.
(3) light path system of the high integration of the present invention's employing carries micro-machine and drives precision displacement table design, compact circuit configuration, and collocation Miniature high-sensitivity spectrometer, narrows down to miniature sizes by instrument overall volume, handled easily.The overall volume and weight configuration of the miniature design of entirety, instrument do a large amount of optimization, achieves miniaturization, portability.
Accompanying drawing explanation
Set forth detection means involved by patent of the present invention and Instrument Design below in conjunction with accompanying drawing and associative operation embodiment, but be not limited to mentioned this several detection means and Instrument Design.
Fig. 1: a kind of integrated described in the embodiment of the present invention 1 can the one-piece construction schematic diagram of imaging type Portable laser Raman spectrum detector;
Fig. 2: a kind of integrated described in the embodiment of the present invention 2 can the integrated optical circuit module diagram of imaging type Portable laser Raman spectrum detector;
Fig. 3: a kind of integrated described in the embodiment of the present invention 3 can the circuit modular structure schematic diagram of imaging type Portable laser Raman spectrum detector;
Fig. 4: a kind of integrated described in the embodiment of the present invention 4 can the micro-imaging CCD photo of imaging type Portable laser Raman spectrum detector;
Fig. 5: a kind of integrated described in the embodiment of the present invention 5 can the sample laser Raman spectroscopy spectrogram of imaging type Portable laser Raman spectrum detector.
Embodiment
Embodiment 1
Fig. 1 is this can the structural representation of imaging Portable laser Raman spectrum detector according to a kind of integrated form of the present invention's design.All parts of instrument are all placed in apparatus frame (1), it is the normal operation position of instrument when vertically placing upward with the detection window (4) being built-in with object lens (10), direct current generator (6) and fine bits moving stage (2) form mechanical shift module, integrated optical circuit module (8) is fixed on fine bits moving stage (2), under the drive of direct current generator (6) and fine bits moving stage (2), integrated optical circuit module (8) is at the 10mm range of motion of vertical direction, thus make the light beam through object lens (10) accurately can focus on the surface of the sample (30) be positioned at above detection window (4), it is that the laser of 785nm wavelength imports integrated optical circuit module (8) navigate on detection window (4) through optical fiber that laser tube (3) sends wavelength, and the sample (30) that detection window (4) is placed above excites the Raman signal of lower generation to import micro spectrometer (5) by integrated optical circuit module (8) through optical fiber at incident light to carry out spectral analysis thus the object realizing detection sample (30) Raman signal.
The power supply of LED white light source (21) and direct current generator (6) is provided by supply module (7).Laser tube (3) and micro spectrometer (5) are directly powered by supporting 12V direct supply.
Embodiment 2
Fig. 2 for the present invention design in the detailed construction schematic diagram of integrated optical circuit module (8).Overall light path is made up of micro-imaging light path and laser Raman spectroscopy excitation-detection light path respectively.
The micro-imaging light path course of work is as follows, by LED white light source (21) outgoing white light vertically from bottom to top planoconvex lens (20) assemble after with the incident angles of 45 degree on half-reflecting half mirror (11), through half-reflecting half mirror (11) reflection after in the horizontal direction with the incident angles of 45 degree to dichroic beamsplitter (R>98%450-764nm, T>88%>789nm) on (12), be irradiated to through detection window (4) after reflected light is vertically focused on by object lens (10) more from bottom to top and be positioned at sample (30) on object lens (10) back focal plane on the surface, the reflected light on sample (30) surface vertically becomes directional light from the top down after object lens (10), then with the incident angles of 45 degree to dichroic beamsplitter (R>98%450-764nm, T>88%>789nm) on (12), reflected light is in the horizontal direction through half-reflecting half mirror (11), focus on convex lens (13) focal imaging on CCD (14), thus white light source can be observed in sample (30) surperficial imaging on CCD (14),
Raman spectrum excites with to detect the light path course of work as follows: by laser tube (3, Fuzhou of China Photop Technologies companies, model: PT20202) laser that sends is by being delivered in light path module (8) by fiber coupler (23) by laser again after Optical Fiber Transmission, expand through extender lens group (15) or become directional light in the horizontal direction, parasitic light is filtered again through bandpass filter (T>90%780 ~ 790nm) (16), then with the incident angles of 45 degree to 785nm double-tone spectroscope (R>98%785nm, T>90%841-1600nm) on (17), reflected light is vertically from bottom to top through dichroic beamsplitter (R>98%450-764nm, T>88%>789nm) (12) transmission, sample (30) is irradiated on the surface through detection window (4) after being focused on by object lens (10) again, the Raman signal that excited sample (30) surface produces is collected via object lens (10), vertically from the top down successively through dichroic beamsplitter (R>98%450-764nm, T>88%>789nm) (12), 785nm double-tone spectroscope (R>98%785nm, T>90%841-1600nm) (17), again through the long pass filter of 785nm (semrock company of the U.S., model: BLP01-785R-25x36, T>90%>812.1nm) (18) filter Rayleigh scattering light, expand through flashlight shaping lens (19) or become directional light, finally by Raman signal fiber coupler (22), Raman signal is transported to micro spectrometer (5, Fuzhou of China Photop Technologies companies, model: PT20007) in carry out data analysis.
Embodiment 3
Fig. 3 is be the electrical block diagram that LED white light source (21) and direct current generator (6) are powered in the present invention, wherein except LED white light source (21) and direct current generator (6), all parts are all integrated in motor and light source power supply module (7).
Motor and light source power supply module (7) are made up of two parts, a part is by the first adjustable voltage reduction module (28, the adjustable voltage reduction module of LM2596S-ADJ DC-DC that Texasinstruments company of the U.S. produces, input voltage 3 ~ 40V, output voltage 1.5 ~ 35V) and LED light source gauge tap (26) composition, LED light source gauge tap (26) is for singly to open double control switch, first adjustable voltage reduction module (28) is by after the conversion of the 12V direct current of input, realizing stable 5V direct current to export, is LED white light source (21) power supply.Another part is by the second adjustable voltage reduction module (29, the adjustable voltage reduction module of LM2596S-ADJ DC-DC that Texasinstruments company of the U.S. produces, input voltage 3 ~ 40V, output voltage 1.5 ~ 35V) and DC MOTOR CONTROL switch (27) composition, DC MOTOR CONTROL switch (27) is for singly to open double control switch, second adjustable voltage reduction module (29) is by after the conversion of the 12V direct current of input, realizing stable 5V direct current to export, is direct current generator (6) power supply.
First adjustable voltage reduction module (28), LED light source gauge tap (26) and LED white light source (21) are connected.By the lighting of LED light source gauge tap (26) control LED white light source (21), to turn off or high low-light level switches.When LED light source gauge tap (26) is set up unlatching, high-ohmic resistor (24) (resistance is 200 ohm) is linked in series loop, and LED white light source (21) is lighted and is low-light level illumination; When centre put by switch (26), no current flows through LED white light source (21), is off state; When LED light source gauge tap (26) puts lower unlatching, low-resistance resistance (25) (resistance is 73 ohm) is linked in series loop, and LED white light source (21) is lighted and is highlight illumination.
Second adjustable voltage reduction module (29), DC MOTOR CONTROL switch (27) and direct current generator (6) are connected.Rising and the decline of direct current generator (6) is controlled by DC MOTOR CONTROL switch (27).Put as operative orientation with instrument integral mirror head erect, when DC MOTOR CONTROL switch (27) is set up unlatching, direct current generator (6) rotates forward, and promotes fine bits moving stage (2) and moves upward; When centre put by DC MOTOR CONTROL switch (27), be off state, direct current generator (6) non rotating, fine bits moving stage (2) is not moved; When lower unlatching put by DC MOTOR CONTROL switch (27), direct current generator (6) reverse rotation, pulls fine bits moving stage (2) to move downward.
Embodiment 4
Fig. 4 is that illustrated device is to CCD (14) microphoto detecting sample (30).Wherein, selected sample (30) is that " micro-fluidic chip " (this chip is the passage that application engraving machine is carved on polymethyl methacrylate organic glass, and with material organic glass on covering, application organic glass thermoset nature, the pipe guiding path that 4 hours form micro-fluidic chip is toasted) at 120 DEG C of temperature, left figure is that laser tube (3) closes the lower microphoto of sample (30) on CCD (14), and right figure is laser tube (3) power stage sample (30) microphoto on CCD (14) when being adjusted to 3mW.Scale as shown in Fig. 4 upper left side is obtained after fixed by micrometering footage number, channel diameter in the micro-image of this sample (30) about 50 μm, in right figure same position microphoto in the laser launched when be laser tube (3) output power being 3mW of circular speck at the laser facula of sample (30) surperficial imaging, spot diameter about 70 μm, can prove thus, the present invention can realize sample (30) inner micro-meter scale location Raman spectrum analysis.
Embodiment 5
Fig. 5 is the Surface enhanced raman spectroscopy passing into the mixed solution of classical silver sol and 4-mercaptopyridine in the micro-fluidic chip sample (30) that obtained by spectrometer (5) of the embodiment of the present invention (6).Be 10 by concentration
-5the 4-mercaptopyridine of mole often liter and classical silver sol (synthetic method list of references: J.Phys.Chem.1982,86,3391-3395) volume ratio 1:9 pumps in the close passage of micro-fluidic chip sample (30) respectively, and in close passage, detects the silver sol enhancing Raman signal of 4-mercaptopyridine with the apparatus in the present invention.By the 785nm wavelength laser that laser instrument (3) sends, light intensity 100mW (after the decay of each assembly of light path, the laser power to sample (30) surface is about 10mW), 10 seconds integral time.Can illustrate that the sensitivity of this apparatus meets the requirement of conventional sense low concentration sample (30) Raman spectrum from the peak intensity of Raman spectrogram.The peak position position of spectrogram is clearly demarcated, from 1009 figure, 1061,1096, the peak position such as 1578 wave numbers can prove that tested substance is 4-mercaptopyridine, thus prove that the wavelength resolution of this instrument meets and analyze requirement.Sample (30) concentration involved by the embodiment of the present invention 6 is low concentration material, by the above-mentioned analysis to Fig. 5, proves that apparatus involved in the present invention meets Portable Raman optical spectrum detector high sensitivity, high-resolution requirement.
Claims (4)
1. integrated, can an imaging type Portable laser Raman spectrum detector, it is characterized in that:
A, be made up of laser tube (3), mechanical shift module, motor and light source power supply module (7), integrated optical circuit module (8) and high-sensitivity miniature spectrometer (5) five part, the common integrated installation of this five part is in apparatus frame (1);
B, mechanical shift module are made up of a DC micromotor (6) and a fine bits moving stage (2), DC micromotor (6) is vertically fixed on the side of fine bits moving stage (2), and integrated optical circuit module (8) is fixed in fine bits moving stage (2);
C, integrated optical circuit module (8) comprise micro-imaging light path and laser Raman spectroscopy excites and gathers light path two parts, micro-imaging light path and laser Raman spectroscopy to be excited and gather light path and integrate by the dichroic beamsplitter (12) in integrated optical circuit module (8);
D, laser Raman spectroscopy excite and gather optical routing extender lens group, bandpass filter, dichroic beamsplitter, focus lens group and object lens and form, the laser sent by laser tube (3) is by being delivered in integrated optical circuit module (8) by fiber coupler (23) by laser again after Optical Fiber Transmission, expand through extender lens group (15) or become directional light in the horizontal direction, parasitic light is filtered again through bandpass filter (16), then with the incident angles of 45 degree on 785nm double-tone spectroscope (17), reflected light is vertically from bottom to top through dichroic beamsplitter (12) transmission, sample (30) is irradiated on the surface through detection window (4) after being focused on by object lens (10) again, sample (30) surface excites the Raman signal of lower generation to collect via object lens (10) at incident light, vertically from the top down successively through dichroic beamsplitter (12), 785nm double-tone spectroscope (17), Rayleigh scattering light is filtered again through the long pass filter of 785nm (18), expand through flashlight shaping lens (19) or become directional light, by optical fiber Raman signal being transported in high sensitive micro spectrometer (5) after Raman signal fiber coupler (22) and carrying out data analysis and process,
E, micro-imaging optical routing LED white light source, focus lens group, half-reflecting half mirror, dichroic beamsplitter, object lens and CCD are formed, by LED white light source (21) outgoing white light vertically from bottom to top planoconvex lens (20) assemble after with the incident angles of 45 degree on half-reflecting half mirror (11), through half-reflecting half mirror (11) reflection after in the horizontal direction with the incident angles of 45 degree on dichroic beamsplitter (12), be irradiated to through detection window (4) after reflected light is vertically focused on by object lens (10) more from bottom to top and be positioned at sample (30) on object lens (10) back focal plane on the surface, the reflected light on sample (30) surface vertically becomes directional light from the top down after object lens (10), then with the incident angles of 45 degree on dichroic beamsplitter (12), reflected light is in the horizontal direction through half-reflecting half mirror (11), focus on convex lens (13) focal imaging on CCD (14), make laser facula at the exact position real time imagery of sample surfaces to CCD, thus realize the positioning analysis of sample.
2. as claimed in claim 1 a kind of integrated, can imaging type Portable laser Raman spectrum detector, it is characterized in that: motor and light source power supply module (7) are made up of two parts, a part is by the first adjustable voltage reduction module (28), LED light source gauge tap (26), high-ohmic resistor (24) and low-resistance resistance (25) composition, LED light source gauge tap (26) is for singly to open double control switch, first adjustable voltage reduction module (28) is by after the conversion of the 12V direct current of input, realize stable 5V direct current to export, for LED white light source (21) power supply, another part is made up of the second adjustable voltage reduction module (29) and DC MOTOR CONTROL switch (27), DC MOTOR CONTROL switch (27) is for singly to open double control switch, second adjustable voltage reduction module (29) is by after the conversion of the 12V direct current of input, realizing stable 5V direct current to export, is direct current generator (6) power supply.
3. as claimed in claim 2 a kind of integrated, can imaging type Portable laser Raman spectrum detector, it is characterized in that: the series connection of the first adjustable voltage reduction module (28), LED light source gauge tap (26) and LED white light source (21); Lighting or turning off by LED light source gauge tap (26) control LED white light source (21); When LED light source gauge tap (26) is set up unlatching, high-ohmic resistor (24) is linked in series loop, and LED white light source (21) is lighted and is low-light level illumination; When centre put by switch (26), no current flows through LED white light source (21), is off state; When LED light source gauge tap (26) puts lower unlatching, low-resistance resistance (25) is linked in series loop, and LED white light source (21) is lighted and is highlight illumination.
4. as claimed in claim 2 a kind of integrated, can imaging type Portable laser Raman spectrum detector, it is characterized in that: the second adjustable voltage reduction module (29), DC MOTOR CONTROL switch (27) and direct current generator (6) are connected, controlled rising or the decline of direct current generator (6) by DC MOTOR CONTROL switch (27); Put as operative orientation with instrument integral mirror head erect, when DC MOTOR CONTROL switch (27) is set up unlatching, direct current generator (6) rotates forward, and promotes fine bits moving stage (2) and moves upward; When centre put by DC MOTOR CONTROL switch (27), be off state, direct current generator (6) non rotating, fine bits moving stage (2) is not moved; When lower unlatching put by DC MOTOR CONTROL switch (27), direct current generator (6) reverse rotation, pulls fine bits moving stage (2) to move downward.
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