CN109187501A - Postposition is divided pupil laser differential confocal LIBS spectrum micro imaging method and device - Google Patents
Postposition is divided pupil laser differential confocal LIBS spectrum micro imaging method and device Download PDFInfo
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
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Abstract
本发明公开的后置分光瞳激光差动共焦LIBS光谱显微成像方法与装置，属于共焦显微成像和光谱成像测量技术领域。本发明将后置分光瞳激光差动共焦显微成像技术与激光诱导击穿光谱探测技术结合，利用经超分辨技术处理的后置分光瞳差动共焦显微镜的微小聚焦光斑对样品进行高空间分辨形态成像，利用光谱探测系统对聚焦光斑激发的激光诱导击穿光谱进行微区光谱探测，利用LIBS光谱探测和后置分光瞳差动共焦探测结构融合实现样品微区完整组分信息与形态参数的高空间分辨和高灵敏成像与探测。本发明可为生物医学、材料科学、矿产、微纳制造等领域形态成像及物质组分探测提供一条全新的有效技术途径。
The invention discloses a post-pupil laser differential confocal LIBS spectral microscopic imaging method and device, which belong to the technical field of confocal microscopic imaging and spectral imaging measurement. The invention combines the post-pupil laser differential confocal microscopy imaging technology with the laser-induced breakdown spectroscopy detection technology, and uses the tiny focusing spot of the post-pupil differential confocal microscope processed by the super-resolution technology to perform high spatial resolution on the sample. Morphological imaging, using the spectral detection system to detect the laser-induced breakdown spectrum excited by the focused spot for micro-area spectral detection, using LIBS spectral detection and post-pupil differential confocal detection structure fusion to achieve complete composition information and morphological parameters of the sample micro-area High spatial resolution and high sensitivity imaging and detection. The invention can provide a brand-new and effective technical approach for morphological imaging and material component detection in the fields of biomedicine, material science, minerals, micro-nano manufacturing and the like.
Description
Technical field
The invention belongs to confocal microscopic imaging technologies, spectral imaging technology technical field, and postposition is divided pupil laser differential
Confocal microscopic imaging technology is combined with laser induced breakdown spectroscopy imaging technique technology, and it is poor to be related to a kind of postposition light splitting pupil laser
Confocal LIBS spectrum micro imaging method and device are moved, in biomedicine, material science, physical chemistry, mineral products, minute manufacturing etc.
Field has wide practical use.
Background technique
The intense pulse laser of laser induced breakdown spectroscopy, which focuses on sample surfaces, can make sample ionization, sample can be excited to produce
Raw plasma can obtain the atom and small molecule element group of sample by the spectrum that detection energy of plasma decline gives off
It is a kind of strong sample component Detection Techniques means at information.
But there are problems following prominent for existing spectrographic detection technology:
1) due to being focused using simple laser come desorption ionization sample, thus its that there are still laser focal beam spots is big, visits
Survey the problems such as spatial resolution is not high；
2) long the time required to light spectrum image-forming, with respect to sample drifting problem often occurs for focal beam spot axial position；
And science is ground in the accurate acquisition of mineral products, " microcell " pattern of space substance and biological sample and component information
Study carefully and produce detection and is all extremely important.In fact, how to detect micro-area composition information with sensitivity is current mine
Produce the important technological problems that the fields such as analysis, biochemistry detection are urgently studied.
Postposition is divided pupil laser differential confocal technology and is detected using illumination and the non-line structure altogether of detection optical path, is not only shown
The azimuthal resolution and Focus accuracy for improving optical path are write, realizes the high-resolution imaging detection of sample topography, and can be effective
Inhibit backscattering interference, improves spectrographic detection signal-to-noise ratio.
Based on this, the present invention proposes that a kind of postposition is divided pupil laser differential confocal LIBS spectrum micro imaging method and dress
It sets, innovation is: pupil laser differential confocal microtechnic and laser will be divided with the postposition of high-space resolution ability for the first time
Induced breakdown spectroscopy (LIBS) technology blends, it can be achieved that sample microcell high-space resolution and highly sensitive pattern and component
Imaging and detection.
A kind of postposition light splitting pupil laser differential confocal LIBS spectrum micro imaging method of the present invention and device can be biology doctor
The pattern component imaging detection in the fields such as, material science, physical chemistry, mineral products, minute manufacturing provide one it is completely new effective
Technological approaches.
Summary of the invention
The purpose of the invention is to improve the spatial resolving power of laser induced breakdown spectroscopy imaging, inhibit imaging process
The drift of middle focal beam spot relative sample, propose a kind of postposition light splitting pupil laser differential confocal LIBS spectrum micro imaging method with
Device, to obtain sample micro-raman spectra information and component information simultaneously.The purpose of the present invention is pass through following technical sides
What case was realized.
Postposition of the invention is divided pupil laser differential confocal LIBS spectrum micro imaging method, utilizes high-space resolution postposition
The focal beam spot of laser differential confocal microscopic system carries out axial fixed-focus and imaging to sample, is visited using laser induced breakdown spectroscopy
The plasma that examining system is divided pupil laser differential confocal microscopic system focal beam spot desorption ionization sample to postposition and generates is sent out
It penetrates spectrum to be detected, sample microcell high-altitude is then then realized with analysis is compared by the fusion of detection data information again
Between differentiate and highly sensitive form and component imaging and detection, comprising the following steps:
Step 1: reflecting collimated light beam simultaneously by compression focal beam spot system, through Amici prism transmission, dichroscope A
It is focused on sample by measurement object lens；
Step 2: computer control precise three-dimensional working platform is made to drive sample attached in measurement object focal point along measuring surface
It closely moves up and down, the light through sample reflection reflects to obtain Returning beam, Returning beam by Amici prism by dichroscope A
After reflection, postposition light splitting pupil measuring beam is formed after the collection pupil filtering in postposition pupil, postposition is divided pupil measuring beam
It converges on dual-quadrant detector by detection object lens, relaying amplifying lens and after relaying amplifying lens, is put about relaying
The first symmetrically placed detection quadrant of big lens axis and the second detection quadrant are split detection to amplification Airy, are ended
In the first microcell of spot the off-axis confocal axial strength curve of strength characteristics first, the strength characteristics of the second microcell of Airy is bent
The off-axis confocal axial strength curve of line second；
It is handled Step 3: the first off-axis confocal axial strength curve and the second off-axis confocal axial strength curve are subtracted each other
It is divided pupil laser differential confocal axial strength curve to postposition, is divided pupil laser differential confocal axial strength curve energy using postposition
Enough it is accurately positioned this of sample axial height information；
Step 4: computer controls three-dimensional according to the dead-center position of postposition light splitting pupil laser differential confocal axial strength curve
Workbench drives sample to move along measuring surface normal direction, focuses on the focal beam spot for measuring object lens 7 on sample；
Step 5: changing collimated light beam light illumination mode, the microcell desorption ionization of sample is excited to generate plasma plume；
Step 6: using the LIBS spectral detector of LIBS spectrum investigating system to being transmitted through dichroscope A and LIBS coupling
It closes the laser induced breakdown spectroscopy signal beams that lens are collected to be detected, measures the sample element group in corresponding focal beam spot region
At information；
Step 7: the laser focal beam spot position sample that computer measures postposition light splitting pupil laser differential confocal detection system
The LIBS spectral information that product elevation information and the laser of LIBS spectrum investigating system detection focus microcell carries out fusion treatment, then
Obtain the height and spectral information of focal beam spot microcell；
Step 8: computer control precise three-dimensional working platform makes to measure the next to be measured of object focal point alignment sample
Then region is operated by step 2~step 7, obtain the height and spectral information of next focal zone to be measured；
Measured Step 9: repeating step 8 until all tested points on sample, then using computer into
Sample shape information and complete component information can be obtained in row processing.
Postposition of the invention is divided pupil laser differential confocal LIBS spectrum micro imaging method, makes parallel described in step 1
Beam shaping is annular beam, the annular beam again through Amici prism transmission, dichroscope A reflection, measurement object lens focus on by
Desorption ionization generates plasma plume in sample.
Postposition of the invention is divided pupil laser differential confocal LIBS spectrum micro imaging method, and the pupil is D type postposition
Pupil or round postposition pupil；Collecting pupil is that D type collects pupil or circular collection pupil；D type postposition pupil and D type collect light
Pupil is used in conjunction with；Round postposition pupil and circular collection pupil are used in conjunction with.
Postposition of the invention is divided pupil laser differential confocal LIBS spectrum micro imaging method, and compression focal beam spot system is used
Generate the vector beam generating system and iris filter substitution of vector beam.
Postposition of the invention is divided pupil laser differential confocal LIBS spectrum microscopic imaging device, including generating excitation beam
Light-source system, Amici prism, the dichroscope A being sequentially placed along light source exit direction are identical as dichroscope A reflection direction
Measurement object lens, precision three-dimensional workbench, dichroscope A reflects the LIBS spectral measurement system of opposite direction, and Amici prism is anti-
Penetrate the postposition light splitting pupil laser differential confocal measuring system and computer processing system in direction.
Postposition of the invention is divided pupil laser differential confocal LIBS spectrum microscopic imaging device, and postposition is divided pupil laser differential
The optional following two mode of confocal detection module is realized:
Mode one, postposition are divided pupil laser differential confocal detecting module by relaying amplifying lens and dual-quadrant detector structure
At wherein the first detection quadrant on dual-quadrant detector test surface and the second detection quadrant are symmetrical about optical axis.
Mode two: postposition light splitting pupil laser differential confocal detecting module is made of relaying amplifying lens, ccd detector,
The first microcell of Airy and the second microcell of Airy that middle ccd detector detects are symmetrical about optical axis.
Postposition of the invention is divided pupil laser differential confocal LIBS spectrum microscopic imaging device, and light-source system is by pulse laser
Device, collector lens, collector lens focal point Optic transmission fiber substitution simultaneously, in laser focusing system introduce outgoing beam decaying
Device introduces detection beam attenuator in postposition light splitting pupil laser differential confocal detection system.By outgoing beam attenuator and spy
Survey beam attenuator constitute Light intensity regulating system, for decay focal beam spot and dual-quadrant detector detection spot intensity, with
Adapt to light intensity demand when sample surfaces positioning.
The utility model has the advantages that
1) " zero crossing " and high-acruracy survey object lens of pupil laser differential confocal axial response curve are divided by postposition
Focus accurately corresponds to this characteristic, realizes accurate fixed-focus to sample, be able to suppress existing spectrometer because long-time spectrum at
Drifting problem of the focal beam spot with respect to sample as in；
2) detection for combining laser induced breakdown spectroscopy, realizes laser induced breakdown spectroscopy component imaging detection and postposition point
The mutual supplement with each other's advantages and structure function fusion of the pattern detection of pupil differential confocal technology, can obtain micro-raman spectra component letter simultaneously
Breath；
3) the preparatory fixed-focus of sample is carried out using " zero crossing " of postposition light splitting pupil laser differential confocal curve, makes minimum focusing
Hot spot focuses on sample surfaces, can be realized sample microcell high-space resolution spectrographic detection and microcell micro-imaging, effectively sends out
Wave the potential differentiated between postposition light splitting pupil laser differential confocal system altitude；
4) using compression focal beam spot technology, it can be improved the spatial resolving power of laser spectrum analyser；
5) signal is obtained due to the method using division focal spot, it can be set on system detection focal plane by changing
The parameter of tiny area is to match the reflectivity of different samples, so as to extend its application field；Calculating can also only be passed through
The matching of the measurement object lens to different NA values is realized in the processing of machine system software, without carrying out any hardware adjustment to system again,
It is advantageously implemented the versatility of instrument.
Detailed description of the invention
Fig. 1 is that postposition of the present invention is divided pupil laser differential confocal LIBS spectrum micro imaging method schematic diagram；
Fig. 2 is that the postposition of the embodiment of the present invention 1 is divided pupil laser differential confocal LIBS spectrum micro imaging method and dress
Set schematic diagram；
Fig. 3 is that the postposition of the embodiment of the present invention 2 is divided pupil laser differential confocal LIBS spectrum micro imaging method and dress
Set schematic diagram；
Fig. 4 is light splitting pupil differential confocal axial strength curve；
Wherein: 1- light-source system, 2- collimation lens, 3- collimated light beam, 4- compression focal beam spot system, 5- Amici prism,
6- dichroscope A, 7- measure object lens, 8- sample, 9- plasma plume, 10- precision three-dimensional workbench, 11-D type postposition pupil,
12-D type collects pupil, 13- detects object lens, 14- postposition light splitting pupil laser differential confocal detection system, 15- relay amplifying lens,
It is micro- that 16- dual-quadrant detector, 17- first detect quadrant, 18- second detects quadrant, 19- amplifies Airy, 20- Airy first
Area, the second microcell of 21- Airy, the off-axis confocal axial strength curve of 22- first, the off-axis confocal axial strength curve of 23- second,
24- is divided pupil laser differential confocal axial strength curve, 25-LIBS spectral signal light beam, 26- decaying light beam, 27- return light
Beam, 28- postposition are divided pupil measuring beam, 29-LIBS spectrum investigating system, 30-LIBS coupled lens, 31-LIBS spectrographic detection
Device, 32- optical fiber incidence end, 33- fiber exit end, 34- computer, 35- vector optical generator, 36- iris filter, 37- circle
Shape postposition pupil, 38- circular collection pupil, 39-CCD detector, 40- pulse laser, 41- collector lens, 42- pass light light
Fibre, 43- outgoing beam attenuator, 44- detect beam attenuator.
Specific embodiment
Invention is further described in detail with reference to the accompanying drawings and examples.
Embodiment 1
Pupil 11 is collected as shown in Figure 1, placing on detection 13 pupil plane of object lens.Light-source system 1 selects point light source, puts light
The excitation beam of source outgoing is by collimation lens 2, compression focal beam spot system 4, Amici prism 5, dichroscope A6 and measurement object
It after mirror 7, converges on sample 8, computer 34 controls precision three-dimensional workbench 10 and drives sample 8 in measurement object lens 7
Near focal point moves up and down, and the light through sample reflection passes through D type postposition by dichroscope A6 reflection, the reflection of Amici prism 5
D type in pupil 11 converges on dual-quadrant detector 16 after collecting pupil 12, detection object lens 13, relaying amplifying lens 14, closes
It is split detection in the first symmetrically placed detection quadrant 17 of acquisition optical axis and second detection 18 pairs of amplification Airy 19 of quadrant,
The strength characteristics for obtaining the first microcell of Airy 20 and the second microcell of Airy 21 are respectively that the first off-axis confocal axial direction is strong
It writes music line 22 and the second off-axis confocal axial strength curve 23；
First off-axis confocal axial strength curve 22 and the second off-axis confocal axial strength curve 23 are subtracted each other processing and obtained
Postposition is divided pupil laser differential confocal axial strength curve 24, is divided pupil laser differential confocal axial strength curve 24 using postposition
This axial height information of sample 8 can be accurately positioned；
Change 1 operating mode of light-source system, improves illumination intensity, the microcell desorption ionization generation of excitation sample 8 etc.
Ion body feathers 9；
Using the LIBS spectral detector 31 of LIBS spectrum investigating system 29 to dichroscope A6 transmission, LIBS coupled lens
The 30 laser induced breakdown spectroscopy signal beams 25 collected are detected, and the sample element composition in corresponding focal beam spot region is measured
Information；
Computer 34 by the laser that measures of postposition light splitting pupil laser differential confocal detection system focus micro-raman spectra information,
The laser induced breakdown spectroscopy information that the laser that LIBS spectrum investigating system 26 detects focuses microcell carries out fusion treatment, is gathered
The height and spectral information of burnt hot spot microcell；
Computer 34, which controls precision three-dimensional workbench 10, to be made to measure next region to be measured that object lens 7 are directed at sample 8,
Then the height and spectral information of next focal zone to be measured are obtained；
Until all tested points on sample 8 are measured, then computer 34 is utilized to carry out data fusion and figure
As reconstruction processing, sample topographical information and complete component information can be obtained.
Embodiment 2
As shown in Fig. 2, compressing focal beam spot system in postposition light splitting pupil laser differential confocal LIBS spectrum microscopic imaging device
System 4 is substituted by vector beam generating system 35, iris filter 36, and D type postposition pupil 11 can be substituted by round postposition pupil 37,
Dual-quadrant detector is substituted by ccd detector 39, and wherein the first microcell of Airy and Airy second of ccd detector detection are micro-
Area, it is symmetrical about optical axis.
Remaining imaging method and process are same as Example 1.
Embodiment 3
As shown in figure 3, point light source 1 can be by arteries and veins in postposition light splitting pupil laser differential confocal LIBS spectrum microscopic imaging device
The substitution of Optic transmission fiber 42 of laser 40, collector lens 41,41 focal point of collector lens is rushed, the light beam that laser 40 is emitted passes through
Collector lens 41 is assembled, and the optical fiber incidence end 32 by being located at 41 focal point of collector lens receives, after the transmission of Optic transmission fiber 42
It is issued by fiber exit end 33 and forms point light source；Meanwhile outgoing beam attenuator 43 is introduced in laser focusing system, in postposition
It is divided in pupil laser differential confocal detection system and introduces detection beam attenuator 44.By outgoing beam attenuator 43 and detection light beam
Attenuator 44 constitutes Light intensity regulating system, and illuminating bundle is modulated to decaying light beam 26 and is used to illuminate, declined by irradiating light beam attenuator 43
Subtract the spot intensity that focal beam spot and dual-quadrant detector 16 detect, to adapt to light intensity demand when sample surfaces positioning.
Remaining imaging method and process are same as Example 1.
A specific embodiment of the invention is described in conjunction with attached drawing above, but these explanations cannot be understood to limit
The scope of the present invention.Protection scope of the present invention is limited by appended claims, any in the claims in the present invention base
Change on plinth is all protection scope of the present invention.
Claims (8)
1. postposition is divided pupil laser differential confocal LIBS spectrum micro imaging method, it is characterised in that: using after high-space resolution
The focal beam spot for setting laser differential confocal microscopic system carries out axial fixed-focus and imaging to sample (8), utilizes laser-induced breakdown
What spectrum investigating system generated postposition light splitting pupil laser differential confocal microscopic system focal beam spot desorption ionization sample (8) etc.
Ionomer emission spectrum is detected, and then then realizes sample with analysis is compared by the fusion of detection data information again
(8) imaging and detection of microcell high-space resolution and highly sensitive form and component, comprising the following steps:
Step 1: collimated light beam (3) is made to transmit (5), dichroscope A by compression focal beam spot system (4), through Amici prism
(6) it reflects and is focused on sample (8) by measurement object lens (7)；
Step 2: computer (34) control precision three-dimensional workbench (10) is made to drive sample (8) along measuring surface in measurement object
Mirror (7) near focal point moves up and down, and the light through sample (8) reflection obtains Returning beam by dichroscope A (6) reflection
(27), Returning beam (27) forms postposition point after Amici prism (5) reflection after the collection pupil filtering in postposition pupil
Pupil measuring beam (28), postposition light splitting pupil measuring beam (28) are by detection object lens (13), relaying amplifying lens (15) and position
It is converged on dual-quadrant detector (16) after relaying amplifying lens (15), it is symmetrically placed about relaying amplifying lens (15) optical axis
The first detection quadrant (17) and the second detection quadrant (18) be split detection to Airy (19) are amplified, obtain Airy the
The off-axis confocal axial strength curve (22) of the strength characteristics first of one microcell (20), the intensity of the second microcell of Airy (22)
The off-axis confocal axial strength curve (23) of characteristic curve second；
Step 3: the first off-axis confocal axial strength curve (22) and the second off-axis confocal axial strength curve (23) are subtracted each other place
Reason obtains postposition light splitting pupil laser differential confocal axial strength curve (24), axially strong using postposition light splitting pupil laser differential confocal
Line (24) of writing music can be accurately positioned sample (8) this axial height information；
Step 4: dead-center position control of the computer (34) according to postposition light splitting pupil laser differential confocal axial strength curve (24)
Three-dimensional working platform (10) drives sample (8) to move along measuring surface normal direction, focuses the focal beam spot for measuring object lens (7)
To on sample (8)；
Step 5: changing collimated light beam (3) light illumination mode, the microcell desorption ionization of excitation sample (8) generates plasma
Plumage (9)；
Step 6: using LIBS spectrum investigating system (29) LIBS spectral detector (31) to through dichroscope A (6) transmission and
The laser induced breakdown spectroscopy signal beams (25) that LIBS coupled lens (30) are collected are detected, and corresponding focal beam spot area is measured
Sample (8) element in domain forms information；
Step 7: the laser focal beam spot position that computer (34) measures postposition light splitting pupil laser differential confocal detection system (14)
Set height of specimen information, the LIBS spectral information for the laser focusing microcell that LIBS spectrum investigating system (29) detects carries out at fusion
Reason, then obtains the height and spectral information of focal beam spot microcell；
Step 8: computer (34) control precision three-dimensional workbench (10) makes to measure object lens (7) focus alignment sample (8)
Next region to be measured, is then operated by step 2~step 7, and the height and light of next focal zone to be measured are obtained
Spectrum information；
Step 9: repetition step 8 is measured until all tested points on sample (8), then computer (34) are utilized
It is handled and obtains sample (8) shape information and complete component information.
2. postposition according to claim 1 is divided pupil laser differential confocal LIBS spectrum micro imaging method, feature exists
In: so that the collimated light beam (3) is shaped as annular beam, the annular beam is again through Amici prism (5) transmission, dichroscope A
(6) it reflects, measurement object lens (7) focuses on desorption ionization on sample (8) and generates plasma plume (9).
3. being divided pupil laser differential confocal LIBS spectrum micro imaging method according to postposition described in right 1, it is characterised in that: institute
Stating pupil is D type postposition pupil (11) or round postposition pupil (37)；Collecting pupil is that D type collects pupil (12) or circular collection
Pupil (38)；D type postposition pupil (11) and D type are collected pupil (12) and are used in conjunction with；Round postposition pupil (37) and circular collection
Pupil (38) is used in conjunction with.
4. postposition according to claim 1 is divided pupil laser differential confocal LIBS spectrum micro imaging method, feature exists
In: compression focal beam spot system (4) is replaced with the vector beam generating system (35) and iris filter (36) for generating vector beam
Generation.
5. postposition is divided pupil laser differential confocal LIBS spectrum microscopic imaging device, it is characterised in that: including generating excitation beam
Light-source system (1), the Amici prism (5), the dichroscope A (6) that are sequentially placed along light source exit direction, with dichroscope A
(6) the identical measurement object lens (7) of reflection direction, precision three-dimensional workbench (10), with dichroscope A (6) reflection opposite direction
The postposition of LIBS spectral measurement system (29), Amici prism (5) reflection direction is divided pupil laser differential confocal measuring system (14)
With computer (34) processing system.
6. postposition according to claim 5 is divided pupil laser differential confocal LIBS spectrum microscopic imaging device, feature exists
In: postposition is divided pupil laser differential detecting module (14) and is made of relaying enlarging objective (15) and dual-quadrant detector (16),
The first detection quadrant (17) and the second detection quadrant (18) on middle dual-quadrant detector (16) test surface is symmetrical about optical axis.
7. a kind of postposition according to claim 5 is divided pupil laser differential confocal LIBS spectrum microscopic imaging device, special
Sign is: postposition is divided pupil laser differential confocal detecting module (14) by relaying amplifying lens (15), ccd detector (39) structure
At the first microcell of Airy (20) and the second microcell of Airy (21) that wherein ccd detector (39) detects are about optical axis pair
Claim.
8. postposition according to claim 5 is divided pupil laser differential confocal LIBS spectrum microscopic imaging device, feature exists
In: light-source system (1) by pulse laser (40), collector lens (41), collector lens (41) focal point Optic transmission fiber (42)
Substitution simultaneously, introduces outgoing beam attenuator (43) in laser focusing system, in postposition light splitting pupil laser differential confocal detection
Detection beam attenuator (44) is introduced in system；Light intensity is constituted by outgoing beam attenuator (43) and detection beam attenuator (44)
Regulating system, for the spot intensity of decay focal beam spot and dual-quadrant detector (16) detection, to adapt to sample surfaces positioning
When light intensity demand.
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| CN115389487A (en) * | 2022-08-08 | 2022-11-25 | 苏州星帆华镭光电科技有限公司 | Method for detecting components and concentration thereof in object |
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