CN109406491A - Body towards liquid sensing detection enhances Raman spectroscopy test device - Google Patents
Body towards liquid sensing detection enhances Raman spectroscopy test device Download PDFInfo
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- CN109406491A CN109406491A CN201811426691.6A CN201811426691A CN109406491A CN 109406491 A CN109406491 A CN 109406491A CN 201811426691 A CN201811426691 A CN 201811426691A CN 109406491 A CN109406491 A CN 109406491A
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- raman
- exciting light
- light
- feedback
- plate
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- 238000001069 Raman spectroscopy Methods 0.000 title claims abstract description 58
- 239000007788 liquid Substances 0.000 title claims abstract description 40
- 238000001514 detection method Methods 0.000 title claims abstract description 33
- 238000012360 testing method Methods 0.000 title claims abstract description 24
- 230000005284 excitation Effects 0.000 claims abstract description 31
- 238000001237 Raman spectrum Methods 0.000 claims abstract description 28
- 230000003595 spectral effect Effects 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 11
- 230000002708 enhancing effect Effects 0.000 claims abstract description 9
- 230000008713 feedback mechanism Effects 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000010453 quartz Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- 239000012530 fluid Substances 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 9
- 230000035945 sensitivity Effects 0.000 abstract description 8
- 230000001965 increasing effect Effects 0.000 abstract description 5
- 239000003403 water pollutant Substances 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- 239000003643 water by type Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000004080 punching Methods 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 239000011888 foil Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000012491 analyte Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000001795 light effect Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Abstract
Body towards liquid sensing detection enhances Raman spectroscopy test device, belongs to the nano-photon device arts of Environment Oriented engineering and sensor technology.It is proposed a kind of three-dimensional Raman spectrum feedback mechanism of building and structure." plate ", " wedge-shaped V plate ", " rectangular pyramid " and " circular cone " shape feedback arrangement are utilized, realizes that the body excitation of Raman spectrum and body are collected.It overcomes previous exciting light and determinand interaction is insufficient, the shortcomings that a large amount of Raman diffused lights are depleted.The intensity of raman spectral signal is significantly increased, to improve the detection sensitivity of object in liquid, the detection for liquid substance such as environment water pollutant provides new technical method, provides technical support for micro content, the detection of low concentration substance.The Raman spectrum feedback device of this body enhancing is applicable not only to laboratory, is equally applicable to the detection of object in the ambient waters such as rivers,lakes and seas.
Description
Technical field
The invention belongs to Environment Oriented engineering and the nano-photon device arts of sensor technology.Construct three-dimensional Raman
Spectrum feedback mechanism and structure realize that the body excitation of Raman spectrum and body are collected, significantly increase the intensity of raman spectral signal, from
And the detection sensitivity of object in liquid is improved, new technical method is provided for the detection of environment water pollutant.
Background technique
Raman spectrum is one based on to the inelastically scattered spectral technique of monochromatic light.It is capable of providing unique " fingerprint
Signal " can test solid-state, liquid, gaseous sample, be the very sensitive and powerful tool of molecular recognition.Improve object
Detection sensitivity, repetitive rate and signal-to-noise ratio are the core contents of correlative study and device development.Especially since the Raman of water
Scattering is very weak, and Raman spectroscopy is the ideal tools for detecting substance in water.
Test liquid is usually to focus into exciting light in liquid, collects scattering light forward or backward, has reported
Many relevant designs and improved method, these methods are mostly with the structure design of probe, light path design, preparation high-performance substrate
It is main.However, a large amount of Raman diffused lights are depleted, and detection sensitivity is low since Raman spectrum excitation, collection efficiency are low.
Different geometries is designed, three-dimensional Raman spectrum feedback mechanism and structure is constructed, Raman spectrum may be implemented
Body excitation and body are collected, and raman spectral signal intensity can be significantly increased, to improve detection sensitivity.For the inspection of liquid
It surveys and new technical method is provided, provide technical support for micro content, the detection of low concentration substance.
Summary of the invention
The present invention is based on the above problems and background technique, propose a kind of body enhancing Raman light of liquid sensing detection
Compose test device.
By constructing three-dimensional Raman spectrum feedback mechanism and structure, realize that the body excitation of Raman spectrum and body are collected, significantly
The intensity for enhancing raman spectral signal, to improve the detection sensitivity of object in liquid.
A kind of body enhancing Raman spectroscopy test device towards liquid sensing detection, which is characterized in that by exciting light
It is incident in solution to be measured, vertical exciting light is put into the three-dimensional Raman spectrum feedback arrangement of geometry, institute in solution to be measured
The three-dimensional Raman spectrum feedback arrangement shape for the geometry stated is selected from " plate " structure, " wedge-shaped V plate ", " rectangular pyramid " and " circle
Cone ", the three-dimensional Raman spectrum feedback arrangement of above-mentioned geometry all has reflection action.
It is further preferred: " plate " structure (attached drawing 1):
" plate " feedback arrangement be in flat substrate covering one layer of metal reflective film, exciting light be incident on be placed in it is to be measured
In flat substrate structure in liquid, exciting light and Raman diffused light are fed back, incident exciting light is perpendicular to the parallel of " plate "
Exciting light or convergence excitation beam.Although the feedback distance for increasing plate feedback will cause raman spectral signal to enhance, too long
Feedback distance will lead to Raman spectral collection efficiency reduction, can be by adjusting the feedback distance of " plate " structure, balanced body
Excitation is collected with body, to reach most strong raman spectral signal intensity.
" wedge-shaped V plate " (attached drawing 2):
" wedge-shaped V plate " is that two planar substrates form V-shaped structure, and it is thin that V-shaped inner structural wall covers one layer of metal reflective
Film constructs feedback arrangement, and exciting light is incident on the metal reflective film, reflects through side wall, feeds back exciting light and Raman scattering
Light constructs three-dimensional feedback mechanism.Exciting light incident direction is parallel with the height of V-shaped, and exciting light is directional light or convergence exciting light
Beam.
" rectangular pyramid " or " circular cone " feedback arrangement (attached drawing 3):
" rectangular pyramid " or " circular cone " feedback arrangement is " rectangular pyramid " or " circular cone " tubular substrat structure, large end face
Opening faces incident exciting light, and the inner wall of " rectangular pyramid " or " circular cone " tubular structure covers one layer of metal reflective film building three
Tie up feedback arrangement.Exciting light is incident on metal reflective film, reflects to form multi-focusing through side wall, multifocal excitation and effectively
Collection Raman diffused light, significantly increase raman spectral signal intensity, constitute three-dimensional feedback mechanism.The direction of exciting light and " four
Pyramid " or the central axis of " circular cone " are parallel, are directional light or convergence excitation beam.
Wedge structure angle (rectangular pyramid or conical taper) and depth can be adjusted according to the actual situation.
Using three-dimensional Raman spectrum feedback arrangement reflected excitation light, excited in the feedback volume that entire laser passes through to be measured
Object generates a large amount of Raman diffused lights, while this feedback arrangement high efficiency collects scattering light, significantly increases raman spectral signal.
Liquid effects mode (attached drawing 4): " rectangular pyramid " and " circular cone " feedback arrangement detection substance Raman light are stated in use
Time spectrum has similar liquid effects mode, with " circular cone " feedback arrangement for example, when not punching substrate, liquid effects side
Formula is shown in Fig. 4 (1) that dotted line direction is liquid flow direction；When punching substrate, liquid effects mode is shown in that Fig. 4 (2), dotted line direction are
Liquid flow direction.
Metal reflective thin-film material is using gold, silver, aluminium, copper to Visible-to-Near InfaRed metal material with high reflectivity.
Exciting light is imported into liquid can be by fiber optic conduction or other optical modules.
Solution to be measured is the fluid sample of the water body of random scale, aqueous solution or non-water quality；It can be examined in laboratory environment
It surveys, also can be made device and be directly protruding into underwater detection, such as rivers,lakes and seas.Object to be checked can be arbitrary in liquid not
With the pollutant in the biology of content, chemical molecular, such as water environment.
Base material can use transparent quartz, glass, organic glass, or the metal using surface polishing.
Advantageous feature of the invention:
1) present invention realizes the body excitation of liquid Raman spectrum, significantly increases Raman signal, and signal amplitude improves
The 1-2 order of magnitude.It overcomes previous exciting light and determinand interacts insufficient disadvantage.
2) three-dimensional feedback arrangement can sufficiently collect Raman diffused light, and a large amount of Raman diffused lights is avoided to be depleted.
3) this body enhancing Raman spectroscopy test device can be obviously improved the sensitivity of target analyte detection, reproducible.
4) feedback arrangement preparation is simple, price economy, material benefit.Reusable, maintenance is simply, conveniently.
5) device is not only suitable for laboratory environment, is also applied for the detection of object in the ambient waters such as rivers,lakes and seas.
6) it can be realized the detection of micro content, low concentration substance.
7) intensity of raman spectral signal is significantly increased, to improve the detection sensitivity of object in liquid, is
The detection of liquid substance such as environment water pollutant provides new technical method, provides for micro content, the detection of low concentration substance
Technical support.The Raman spectrum feedback device of this body enhancing is applicable not only to laboratory, is equally applicable to the rings such as rivers,lakes and seas
The detection of object in the water of border.
Detailed description of the invention
The diagrammatic cross-section of Fig. 1, " plate " feedback arrangement.
Wherein (1) the corresponding index path for parallel excitation beam；(2) the corresponding index path for convergence excitation beam；
A (solid line): parallel excitation beam；B (dotted line): the Raman diffused light being collected into；C: flat substrate；D: metal foil
Film；E (solid line): convergence excitation beam；F (dotted line): the Raman diffused light being collected into.
The diagrammatic cross-section of Fig. 2, " wedge-shaped V plate " feedback arrangement；
Wherein (1) corresponding 3D for " wedge-shaped V plate " feedback arrangement schemes；(2) the corresponding optical path for parallel excitation beam
Figure；(3) the corresponding index path for convergence excitation beam；
A (solid line): parallel excitation beam；B (dotted line): the Raman diffused light being collected into；C: wedge-shaped substrate；D: metal foil
Film；E (solid line): convergence excitation beam；F (dotted line): the Raman diffused light being collected into.
The 3D of Fig. 3, " rectangular pyramid " and " circular cone " feedback arrangement scheme and diagrammatic cross-section.
The wherein 3D figure of (1) " rectangular pyramid " feedback arrangement；(2) and the 3D of " circular cone " feedback arrangement schemes；(3) " rectangular pyramid " and
The corresponding parallel exciting light schematic diagram of " circular cone " feedback arrangement section；(4) " rectangular pyramid " and " circular cone " feedback arrangement section is corresponding
Convergence exciting light schematic diagram；
A (solid line): parallel excitation beam；B (dotted line): the Raman diffused light being collected into；C: substrate；D: metallic film；E
(solid line): convergence excitation beam；F (dotted line): the Raman diffused light being collected into.
Fig. 4, liquid effects schematic diagram.
(1) " circular cone " feedback arrangement liquid effects schematic diagram of substrate is not punched；(2) " circular cone " for punching substrate is anti-
Present structured liquids mode of action schematic diagram.
Fig. 5, alcohol Raman spectrum.
(a) test of corresponding embodiment 2, (b) test of corresponding embodiment 3；(c) test of corresponding embodiment 4.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but the present invention is not limited to following embodiments.
Embodiment 1: the preparation of " plate " feedback arrangement and body enhancing Raman spectroscopy test device and method.
(1) 10 × 10mm is cleaned2Quartz plate it is spare.
(2) gold-plated with vacuum vapour deposition, the golden film that thickness is greater than 100nm is prepared on above-mentioned quartz plate.See Fig. 1 (D).
(3) exciting light that wavelength is 785nm is focused on and contains spirituous quartz cell waist, focal length 50.8mm, laser
Power is 150mW.
(4) it is placed perpendicular to exciting light and obtains the quartz plate for being covered with golden film in (2), be used as " plate " and feed back.
(5) under centainly excitation liquid thickness, time of integration 3s is tested and is stored Raman spectrum.
Embodiment 2: whether there is the alcohol Raman spectrum comparison of " plate " feedback.
(1) referring to embodiment 1, but plate feedback is not added, stores the raman spectral signal measured at this time, for without feedback Raman
Signal.See Fig. 5 (a) dotted line.
(2) vertical exciting light places plate feedback, moves plate feedback arrangement along laser direction, and distance is fed back in adjustment,
9.5mm obtains most strong Raman signal peak intensity after focus.The raman spectral signal measured at this time is stored, feeds back Raman letter for plate
Number.See Fig. 5 (a) solid line.
(3) test result twice is compared, tests alcohol using plate feedback arrangement, raman spectral signal intensity is no feedback
2.6 times when test.
Embodiment 3: difference feedback changes apart from Raman spectrum.
(1) referring to embodiment 1, plate feedback arrangement, adjustment feedback distance, it can be observed that drawing are moved along excitation light direction
Graceful spectral signal peak intensity increases with feedback distance and is enhanced, plate feedback once be more than position at 9.5mm after focus, intensity with
Distance increases and declines.
(2) raman spectral signal after focus, focus after 9.5mm and focus at the position 13mm is had recorded respectively.See Fig. 5
(b)。
Embodiment 4: difference excitation changes apart from Raman spectrum.
(1) referring to embodiment 1, pivotal plate structure is incident on exciting light on plate feedback arrangement in 45° angle, incident
Light is emitted in 90 ° from prepare liquid after flat reflective, to allow have the liquid portion laser of laser excitation and determinand phase
Interaction, and can not interact with determinand after plate since exciting light is reflected determinand, form truncation exciting light
Effect.The slab construction is moved along laser direction, raman spectral signal peak intensity increases with excitation distance to be gradually increased, Zhi Daoda
The Raman signal intensity tested when to without truncation.
(2) 5mm before focus, the raman spectral signal after focus and focus at the position 5mm are had recorded respectively.See Fig. 5 (c).
Claims (9)
1. a kind of body towards liquid sensing detection enhances Raman spectroscopy test device, which is characterized in that enter exciting light
It is mapped in solution to be measured, vertical exciting light is put into the three-dimensional Raman spectrum feedback arrangement of geometry in solution to be measured, described
Geometry three-dimensional Raman spectrum feedback arrangement shape be selected from " plate " structure, " wedge-shaped V plate ", " rectangular pyramid " and " justify
Cone ", the three-dimensional Raman spectrum feedback arrangement of above-mentioned geometry all has reflection action.
2. a kind of body towards liquid sensing detection described in accordance with the claim 1 enhances Raman spectroscopy test device,
It is characterized in that, " plate " feedback arrangement is that one layer of metal reflective film of covering, exciting light are incident on the plate in flat substrate
In structure, which feeds back exciting light and Raman diffused light, and incident exciting light is the parallel exciting light of vertical " plate "
Or convergence excitation beam.
3. a kind of body towards liquid sensing detection described in accordance with the claim 1 enhances Raman spectroscopy test device,
It is characterized in that, wedge-shaped V plate is that two planar substrates form V-shaped structure, and V-shaped inner structural wall covers one layer of metal reflective film
Feedback arrangement is constituted, exciting light is incident on the metal reflective film, parallel, the wedge-shaped V of height of exciting light incident direction and V-shaped
Plate structural feedback exciting light and Raman diffused light, exciting light are directional light or convergence excitation beam.
4. a kind of body towards liquid sensing detection described in accordance with the claim 1 enhances Raman spectroscopy test device,
It is characterized in that, " rectangular pyramid " or " circular cone " feedback arrangement are " rectangular pyramid " or " circular cone " tubular substrat structure, the opening of large end face
Incident exciting light is faced, the inner wall of " rectangular pyramid " or " circular cone " tubular structure covers one layer of metal reflective film and constitutes feedback knot
Structure；Exciting light is incident on metal reflective film, reflects to form multi-focusing through side wall, multifocal excitation and effective collect are drawn
Graceful scattering light significantly increases Raman scattered light intensity, constitutes three-dimensional feedback mechanism；The direction of exciting light and " rectangular pyramid " or " circle
The central axis of cone " is parallel, is directional light or convergence excitation beam.
5. according to a kind of described in any item body enhancing Raman spectrum tests towards liquid sensing detection of claim 2-4
Device, which is characterized in that metal reflective film selects one of gold, silver, aluminium, copper.
6. a kind of body towards liquid sensing detection described in accordance with the claim 1 enhances Raman spectroscopy test device,
It is characterized in that, exciting light, which is imported into liquid, passes through fiber optic conduction.
7. a kind of body towards liquid sensing detection described in accordance with the claim 1 enhances Raman spectroscopy test device,
It is characterized in that, solution to be measured is the fluid sample of the water body of random scale, aqueous solution or non-water quality.
8. a kind of body towards liquid sensing detection described in accordance with the claim 1 enhances Raman spectroscopy test device,
It is characterized in that, base material uses transparent quartz, glass, organic glass, or the metal using surface polishing.
9. the method for carrying out body enhancing Raman spectrum test using device described in claim 1, which is characterized in that utilize three-dimensional
Raman spectrum feedback arrangement reflected excitation light generates a large amount of Raman diffused lights, while this is anti-in the volume that entire laser passes through
Feedback structure, which helps to improve, collects Raman scattering light efficiency, significantly increases raman spectral signal.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811426691.6A CN109406491A (en) | 2018-11-27 | 2018-11-27 | Body towards liquid sensing detection enhances Raman spectroscopy test device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811426691.6A CN109406491A (en) | 2018-11-27 | 2018-11-27 | Body towards liquid sensing detection enhances Raman spectroscopy test device |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010117226A (en) * | 2008-11-12 | 2010-05-27 | Ricoh Co Ltd | Raman spectrometric measuring instrument and method for measurement |
| CN102156114A (en) * | 2010-02-12 | 2011-08-17 | 财团法人工业技术研究院 | Raman detection method and system |
| JP2012242245A (en) * | 2011-05-19 | 2012-12-10 | Horiba Ltd | Raman scattering light detection device |
| CN205719979U (en) * | 2016-04-11 | 2016-11-23 | 北京大学 | In a kind of liquid, induced with laser strengthens detection and the sorting unit of Raman spectrum |
| CN107703117A (en) * | 2017-10-31 | 2018-02-16 | 上海化工研究院有限公司 | A kind of Raman spectrum probe extension apparatus for being used in liquid detect |
| CN209446469U (en) * | 2018-11-27 | 2019-09-27 | 北京工业大学 | Body towards liquid sensing detection enhances Raman spectroscopy test device |
-
2018
- 2018-11-27 CN CN201811426691.6A patent/CN109406491A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010117226A (en) * | 2008-11-12 | 2010-05-27 | Ricoh Co Ltd | Raman spectrometric measuring instrument and method for measurement |
| CN102156114A (en) * | 2010-02-12 | 2011-08-17 | 财团法人工业技术研究院 | Raman detection method and system |
| JP2012242245A (en) * | 2011-05-19 | 2012-12-10 | Horiba Ltd | Raman scattering light detection device |
| CN205719979U (en) * | 2016-04-11 | 2016-11-23 | 北京大学 | In a kind of liquid, induced with laser strengthens detection and the sorting unit of Raman spectrum |
| CN107703117A (en) * | 2017-10-31 | 2018-02-16 | 上海化工研究院有限公司 | A kind of Raman spectrum probe extension apparatus for being used in liquid detect |
| CN209446469U (en) * | 2018-11-27 | 2019-09-27 | 北京工业大学 | Body towards liquid sensing detection enhances Raman spectroscopy test device |
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