CN107907526B - Deep space detection micro-region self-adaptive Raman fluorescence imaging combined system - Google Patents
Deep space detection micro-region self-adaptive Raman fluorescence imaging combined system Download PDFInfo
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- CN107907526B CN107907526B CN201711426271.3A CN201711426271A CN107907526B CN 107907526 B CN107907526 B CN 107907526B CN 201711426271 A CN201711426271 A CN 201711426271A CN 107907526 B CN107907526 B CN 107907526B
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- 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
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- 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
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
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- 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
- G01N21/84—Systems specially adapted for particular applications
Abstract
The invention discloses a deep space detection micro-area self-adaptive Raman fluorescence imaging combined system which consists of a main controller, a spectrometer, an optical fiber, a three-dimensional motor driver, a three-dimensional precise electric platform and an optical head. The invention has the beneficial effects that the invention provides a self-adaptive Raman fluorescence imaging combined system, which can adaptively adjust the diameter of a focusing light spot during micro-area analysis; taking the average gray scale of the area of the electronic ocular as the intensity of a scanning imaging point, and simultaneously meeting the requirements of self-focusing and wide-spectrum scanning imaging; the three-dimensional space active laser Raman, hyperspectral fluorescence and visible broad spectrum scanning imaging can be realized simultaneously, and various information can be provided for micro-area analysis.
Description
Technical Field
The invention relates to a material detection system, in particular to a material detection system adopting scanning laser Raman imaging, scanning laser-induced fluorescence imaging and area array broad spectrum scanning imaging, which is suitable for detecting materials in a deep space detection planetary open environment and belongs to the field of planetary in-situ detection.
Background
For future deep space exploration, higher requirements are put on substance component detection technology and method, and in-situ fine detection capability is a high-point technology aimed by various aerospace countries. The fine detection requires smaller laser focus point, small analyzed substance quantity, richer element and molecular species, more accurate quantification and is carried out under the monitoring of extremely high spatial resolution imaging.
Laser Raman (Raman) and ultraviolet laser induced fluorescence are important means for analysis of material components, wherein laser Raman can be used for analysis of material molecular composition, and ultraviolet laser induced fluorescence can be used for analysis of some elements, especially rare earth elements, besides imaging. The analysis of Raman substances in deep space exploration has higher requirements than the conventional Raman application, and the main challenges and technical difficulties are that the particle size of the same mineral particles is extremely small due to the complex composition of minerals contained in the rock and soil of the tested object. Therefore, when in micro-area analysis, the laser focusing light spot is required to be in the order of 1 micron, so that the mineral can be accurately subjected to micro-area analysis, the requirement on a microscopic optical path is extremely high, the conventional Raman probe is influenced by an optical fiber transmission mode, and the focusing light spot is influenced by the degradation of the laser mode and the diffraction limit, so that the focusing light spot is often larger than 5 microns, and the requirement cannot be met; the combination of the free light path, the short wavelength laser and the high-magnification high-numerical aperture microscope objective lens can theoretically obtain a very small focusing light spot, but because the focusing depth of field is very small, a proper self-focusing scheme for analyzing the three-dimensional structure of the micro-area analysis must be found, the focusing light spot of each point is ensured to be consistent in size and to be consistent with a design value, and meanwhile, if the self-focusing time is long, the scanning imaging speed is influenced. Therefore, a simple and rapid raman self-focusing and broad-spectrum scanning imaging method is required.
Aiming at the requirements of deep space micro-area Raman detection and imaging, the invention provides a substance detection system adopting scanning laser Raman imaging, scanning laser-induced fluorescence imaging and area array broad spectrum scanning imaging, which is suitable for micro-area substance detection in a deep space detection planetary open environment, and can obtain the three-dimensional morphology of micro-area and the corresponding molecular distribution and rare earth fluorescent substance distribution.
Disclosure of Invention
The invention aims to provide a deep space detection micro-region self-adaptive Raman fluorescence imaging combined system, which can accurately obtain the required constant focusing light spot size, and obtain the micro-region three-dimensional morphology of a detection object while detecting the Raman fluorescence spectrum distribution, thereby meeting the requirements of micro-region in-situ material analysis.
The self-adaptive Raman fluorescence imaging combined system provided by the invention consists of a main controller, a spectrometer, an optical fiber, a three-dimensional motor driver, a three-dimensional precise electric platform and an optical head;
the optical head consists of an ultraviolet Raman laser, an ultraviolet interference filter, a secondary motor driver, a secondary linear electric platform, a low-power ultraviolet microscope objective, a dichroic mirror, a long-working-distance high-power ultraviolet microscope objective, a main motor driver, a main linear electric platform, an ultraviolet Rayleigh filter, a proportional beam splitter, a microscope objective, a tube lens and an electronic eyepiece; an imaging lens and an image sensor are arranged in the electronic ocular;
the cylindrical near-collimation laser beam emitted by the ultraviolet Raman laser along the main optical axis passes through the ultraviolet interference filter, so that the frequency-division harmonic interference of the ultraviolet laser emitted by the ultraviolet Raman laser can be filtered, and the signal-to-noise ratio of the Raman signal excited by the ultraviolet Raman laser is higher; the cylindrical near-collimation laser beam passes through the ultraviolet interference filter and then passes through the low-power ultraviolet microscope objective lens to form a conical laser beam; after passing through the dichroic mirror, the conical laser beam reaches the entrance pupil of the long working distance high-power ultraviolet microscope objective, and at the position of the entrance pupil, the diameter of the conical laser beam is larger than the diameter of the entrance pupil, and as the cone angle of the conical laser beam is a fixed value, the farther the distance between the low-power ultraviolet microscope objective and the long working distance high-power ultraviolet microscope objective is, the larger the diameter of the conical laser beam is than the diameter of the entrance pupil, the weaker the laser energy passing through the long working distance high-power ultraviolet microscope objective is, but the smaller the focusing light spot is; therefore, the distance between the low-power ultraviolet microscope objective and the long-working distance high-power ultraviolet microscope objective can be adjusted to make a trade-off between the laser energy passing through the long-working distance high-power ultraviolet microscope objective and the focused light spot size, namely, the large energy and the large light spot and the small energy and the small light spot; the echo signal reversely passes through the high-power ultraviolet microscope objective lens with a long working distance along the main optical axis, and after being reflected by the bicolor lens, the echo signal advances along the receiving optical axis and is divided into two orthogonal paths after reaching the proportional beam splitter: one path of the reflected light travels along an imaging optical axis, is focused between one time and two times of focal length of an imaging lens in an electronic eyepiece through a tube lens, and forms an amplified real image to an image sensor through the imaging lens; the other path of the light passes through the proportional light splitting sheet, is subjected to Rayleigh scattering filtering of ultraviolet Raman laser wavelength by the ultraviolet Rayleigh filter, is focused to the incident end face of the optical fiber by the microscope objective, and then enters the spectrometer for analysis; the low-power ultraviolet microscope objective is arranged on the secondary linear electric platform and can carry out one-dimensional precise translation along the main optical axis under the drive of the secondary motor driver; the long working distance high-power ultraviolet microscope objective is arranged on the main linear electric platform and can carry out one-dimensional precise translation along the main optical axis under the drive of the main motor driver; the translation of the secondary linear electric platform is mainly used for changing the distance between the low-power ultraviolet microscope objective and the long-working-distance high-power ultraviolet microscope objective; the translation of the main linear electric platform is mainly used for accurately focusing the high-power ultraviolet microscope objective lens with a long working distance; the main optical axis, the imaging optical axis and the receiving optical axis are coplanar; the main optical axis is parallel to the imaging optical axis and perpendicular to the receiving optical axis;
the optical head is arranged on a three-dimensional precise electric platform which can perform submicron-level three-dimensional precise movement under the drive of a three-dimensional motor driver;
the main controller can send control instructions to the three-dimensional motor driver, the main motor driver, the secondary motor driver, the ultraviolet Raman laser, the image sensor and the spectrometer; and can receive the output digital image of the image sensor and the output spectrum information of the spectrometer;
the self-adaptive Raman fluorescence imaging combined method provided by the invention comprises the following steps:
(1) Adaptive focal spot calibration for an intended focal spot
In the in-situ detection of deep space substances, different scale Raman focal points, namely expected focal spots, are required for different detection objects, for example, for minerals with more uniform distribution, expected focal spots with slightly larger sizes can be adopted; for minerals with more variation, the expected focal spot with very small size can be adopted to realize very fine micro-area analysis;
firstly, setting the diameter of an expected focal spot according to the basic property of a detection object of a test area; placing a measurement reticle in a test area below the long working distance high power ultraviolet microscope objective; a measurement reticle is provided with uniform scribing lines;
the main controller controls the starting of the ultraviolet Raman laser, and the ultraviolet laser beam emitted by the main controller sequentially passes through the ultraviolet interference filter, the low-power ultraviolet microscope objective and the dichroic mirror, and then is illuminated and focused to the measurement reticle through the high-power ultraviolet microscope objective with a long working distance to form a real-time focal spot; the reflected light of the measuring reticle passes through the high-power ultraviolet microscope objective lens with long working distance along the main optical axis in the reverse direction, is reflected by the bicolor mirror, is reflected by the proportional beam splitter, is focused by the tube lens, and is subjected to real-time microscopic imaging to the image sensor by the imaging lens;
the main controller receives the microscopic digital image output by the image sensor and performs real-time image processing; acquiring the excircle profile of the real-time focal spot by adopting an edge extraction algorithm, thereby determining an imaging area of the real-time focal spot, and calculating the average gray value G of all pixels in the imaging area;
the main controller sends out an instruction to the main motor driver to drive the main linear electric platform to move downwards by one step; the main controller receives microscopic digital images output by the image sensor, determines an imaging area of a real-time focal spot, calculates an average gray value G of all pixels in the imaging area, and compares whether the G value is increased or decreased: if the G value increases, it indicates that the downward movement is in a direction approaching the focus; if the G value decreases, it indicates that the upward movement is in a direction approaching the focus;
the main controller sends out an instruction to the main motor driver to drive the main linear electric platform to move towards the direction close to the focus, and simultaneously calculates the average gray value G of all pixels in the imaging area of the real-time focal spot in real time until the G value reaches the maximum value, and the main controller sends out an instruction to the main motor driver to stop moving in the tight focusing state;
in a tight focusing state, the main controller acquires the linear position of a reticle of a measurement reticle and the excircle contour of a real-time focal spot by adopting an edge extraction algorithm on a microscopic digital image output by an image sensor, and then calculates the number of pixels at intervals of adjacent reticles and the number of pixels of the excircle contour diameter of the real-time focal spot, so that the diameter of the real-time focal spot is calculated according to the spacing of the reticles;
if the diameter of the real-time focal spot is larger than the diameter of the expected focal spot, the main controller sends a command to the secondary motor driver to drive the secondary linear electric platform to move upwards, the distance between the low-power ultraviolet microscope objective and the long-power ultraviolet microscope objective with a high working distance is increased, at the moment, the laser energy passing through the long-power ultraviolet microscope objective with a high working distance is weakened, but the real-time focal spot is reduced until the diameter of the real-time focal spot is equal to the diameter of the expected focal spot, and the main controller sends a command to the secondary motor driver to stop the movement of the secondary linear electric platform;
similarly, if the diameter of the real-time focal spot is smaller than the diameter of the expected focal spot, the main controller sends an instruction to the secondary motor driver to drive the secondary linear electric platform to move downwards, the distance between the low-power ultraviolet microscope objective and the long-power ultraviolet microscope objective is reduced, at the moment, the laser energy passing through the long-power ultraviolet microscope objective is increased, the real-time focal spot is increased until the diameter of the real-time focal spot is equal to the diameter of the expected focal spot, and the main controller sends an instruction to the secondary motor driver to stop the movement of the secondary linear electric platform;
(2) Single point tight focusing of detected object
Removing the measurement reticle, and moving the self-adaptive Raman fluorescence imaging combined system into an actual test area, wherein the detection object is positioned below the optical head, and the distance from the long working distance high-power ultraviolet microscope objective is far greater than the focal length of the long working distance high-power ultraviolet microscope objective;
the main controller controls and starts the ultraviolet Raman laser, ultraviolet laser beams emitted by the ultraviolet Raman laser sequentially pass through the ultraviolet interference filter, the low-power ultraviolet microscope objective and the dichroic mirror, then the ultraviolet laser beams are defocused to the surface of a detection object through the long-working-distance high-power ultraviolet microscope objective, reflected light passes through the long-working-distance high-power ultraviolet microscope objective along a main optical axis in the reverse direction, is reflected by the dichroic mirror, is reflected by the proportional beam splitter, is focused by the tube lens, and is subjected to real-time microscopic imaging to the image sensor through the imaging lens; the main controller receives the microscopic digital image output by the image sensor and performs fast Fourier transform to extract the high-frequency component H;
the main controller sends an instruction to the three-dimensional motor driver to drive an optical head on the three-dimensional precise electric platform to move downwards along the Z axis, at the moment, the distance between a detected object and a long working distance high-power ultraviolet microscope objective lens is reduced, in the moving process, the main controller continuously carries out fast Fourier transform on a microscopic digital image output by the image sensor in real time, and continuously extracts a high-frequency component H until the H reaches the maximum value, at the moment, laser is tightly focused to one point on the surface of the detected object, the size of a real-time focal spot is equal to the size of an expected focal spot, and at the moment, the laser is in a tightly focused state;
(3) Raman fluorescence and imaging information acquisition
In this tightly focused state, the main controller records the three-dimensional displacement of the three-dimensional precision motorized stage, and sets it as the initial three-dimensional coordinate (x 1 ,y 1 ,z 1 ) The method comprises the steps of carrying out a first treatment on the surface of the The main controller receives microscopic digital images output by the image sensor, acquires the excircle profile of the real-time focal spot by adopting an edge extraction algorithm, thereby determining the imaging area of the real-time focal spot, and calculating the average gray value g of all pixels in the imaging area 1 The method comprises the steps of carrying out a first treatment on the surface of the Raman and fluorescence backscattering of the real-time focal spot position on the surface of the detection object passes through a high-power ultraviolet microscope objective lens with a long working distance along a main optical axis, is reflected by a bicolor mirror, passes through a proportional beam splitter, filters Rayleigh scattering of the wavelength of an ultraviolet Raman laser by an ultraviolet Rayleigh filter, is focused on the incident end face of an optical fiber by the microscope objective lens, and then enters a spectrometer, and the spectrometer outputs a spectrum signal to a main controller for analysis; the main controller firstly extracts n discrete Raman spectrum lines lambda of the spectrum signal 1 ，λ 2 ，λ 3 ，...，λ n Record the spectral line intensity I 11 ，Ι 12 ，Ι 13 ，...，Ι 1n The method comprises the steps of carrying out a first treatment on the surface of the Then dividing the continuous fluorescence spectrum line into m sections with equal spectral intervals; and recording the average intensity J of the fluorescence spectrum of each segment 11 ，J 12 ，J 13 ，...，J 1m ；
(4) Scanning micro-area analysis
The main controller determines the number of scanning points A, B in the XY direction of the micro-area analysis and the scanning step C, D; the main controller sends out an instruction to the three-dimensional motor driver to drive the optical head on the three-dimensional precise electric platform to perform S-shaped scanning of an XY plane, and the single-point tight focusing in the step (2) is executed for each point on the XY plane and then moves up and down along a Z axis;
for each scanning point i (i is more than or equal to 2 until i is equal to A multiplied by B), in the tight focusing state of the point, the main controller records the three-dimensional displacement of the three-dimensional precision electric platform and determines the three-dimensional coordinates (x i ,y i ,z i ) The method comprises the steps of carrying out a first treatment on the surface of the The main controller receives microscopic digital images output by the image sensor, acquires the excircle profile of the real-time focal spot by adopting an edge extraction algorithm, thereby determining the imaging area of the real-time focal spot, and calculating the average gray value g of all pixels in the imaging area i The method comprises the steps of carrying out a first treatment on the surface of the The main controller records n discrete Raman spectrum lines lambda 1 ，λ 2 ，λ 3 ，...，λ n Line intensity I) i1 ，Ι i2 ，Ι i3 ，...，Ι in The method comprises the steps of carrying out a first treatment on the surface of the And recording the average intensity J of the fluorescence spectrum of each section of the m sections of the fluorescence spectrum i1 ,J i2 ,J i3 ,...,J im ；
The main controller firstly synthesizes three-dimensional coordinates of A multiplied by B scanning points, and draws the three-dimensional geometric morphology of the surface of the detection object of the scanning area; then, g of each scanning point is integrated 1 ,g 2 ,...,g i ,., a gray scale image of the three-dimensional geometry of the surface of the object to be detected can be obtained; then, the I of each scanning point is integrated 11 ,I 21 ,...,I i1 ,., the wavelength of the surface of the object to be inspected is lambda 1 Similarly, the I of each scanning point is integrated 12 ,I 22 ,...,I i2 ,., the wavelength of the surface of the object to be inspected is lambda 2 Is a raman image of the surface of the object until the wavelength of the surface of the object to be detected is λ n Raman image of (a); finally, integrating J of each scanning point 11 ,J 21 ,...,J i1 ,. obtaining a fluorescence image of a first spectral band of the surface of the object under investigation, similarly integrating the J's of the individual scan points 12 ,J 22 ,...,J i2 ,., obtaining a fluorescence image of a second spectral band of the surface of the object to be detected, until a fluorescence image of an m-th spectral band of the surface of the object to be detected is obtained;
thus, the micro-region analysis is completed, and three-dimensional morphology distribution of the micro-region, and wide-spectrum images of A multiplied by B scanning points, ultraviolet laser Raman images of n wavelengths and ultraviolet laser-induced fluorescence hyperspectral images of m spectral bands on the three-dimensional morphology distribution are obtained.
The invention has the beneficial effects that the invention provides a self-adaptive Raman fluorescence imaging combined system, which can adaptively adjust the diameter of a focusing light spot during micro-area analysis; taking the average gray scale of the area of the electronic ocular as the intensity of a scanning imaging point, and simultaneously meeting the requirements of self-focusing and wide-spectrum scanning imaging; the three-dimensional space active laser Raman, hyperspectral fluorescence and visible broad spectrum scanning imaging can be realized simultaneously, and various information can be provided for micro-area analysis.
Drawings
FIG. 1 is a schematic diagram of a system structure according to the present invention, wherein: 1-three-dimensional motor driver; 2—an optical head; 3-ultraviolet raman laser; 4-a primary optical axis; 5-an ultraviolet interference filter; 6-a secondary motor drive; 7-a master controller; 8-Low power ultraviolet microscope objective; 9—a secondary linear electric platform; 10—imaging optical axis; 11-electronic eyepiece; 12—a spectrometer; 13—optical fiber; 14—a microobjective; 15—a receiving optical axis; 16-an ultraviolet rayleigh filter; 17—a proportional beam splitter; 18—real-time focal spot; 19-the intended focal spot; 20-scribing; 21—a main motor driver; 22-a main linear electric platform; 23—probing objects; 24-measurement reticle; 25-long working distance high power ultraviolet microscope objective; 26—entrance pupil; 27—a dichroic mirror; 28-a cone laser beam; 29—a three-dimensional precision electric platform; 30—a cylindrical near collimated laser beam; 31—an image sensor; 32—imaging lens; 33-tube lens.
Detailed Description
An embodiment of the present invention is shown in fig. 1.
The self-adaptive Raman fluorescence imaging combined system provided by the invention consists of a main controller 7, a spectrometer 12, an optical fiber 13, a three-dimensional motor driver 1, a three-dimensional precise electric platform 29 and an optical head 2;
the optical head 2 consists of an ultraviolet Raman laser 3, an ultraviolet interference filter 5, a secondary motor driver 6, a secondary linear electric platform 9, a low-power ultraviolet microscope objective 8, a bicolor mirror 27, a long working distance high-power ultraviolet microscope objective 25, a main motor driver 21, a main linear electric platform 22, an ultraviolet Rayleigh filter 16, a proportional beam splitter 17, a microscope objective 14, a tube lens 33 and an electronic eyepiece 11; the electronic eyepiece 11 is internally provided with an imaging lens 32 and an image sensor 31;
the cylindrical near-collimated laser beam 30 emitted by the ultraviolet raman laser 3 (in this embodiment, a continuous laser with 360nm and 50 mW) along the main optical axis 4 passes through the ultraviolet interference filter 5 (the ultraviolet interference filter 5 is an ultraviolet narrow-band filter, in this embodiment, a band-pass filter with 360nm and a bandwidth of 1 nm), so that the frequency-division harmonic interference of the ultraviolet laser emitted by the ultraviolet raman laser 3 can be filtered, and the signal-to-noise ratio of the excited raman signal is higher; after passing through the ultraviolet interference filter 5, the cylindrical near-collimated laser beam 30 passes through the low-power ultraviolet microscope objective 8 to form a conical laser beam 28; after passing through the dichroic mirror 27 (high transmittance at 360nm and high reflectance at 364nm in this embodiment), the cone-shaped laser beam 28 reaches the entrance pupil 26 of the long working distance high power ultraviolet microscope objective 25 (the infinite compound flat field aberration eliminating ultraviolet 100X microscope objective is adopted in this embodiment, the ultra-long working distance is 11 mm), and at the position of the entrance pupil 26, the diameter of the cone-shaped laser beam 28 is larger than that of the entrance pupil 26, and because the cone angle of the cone-shaped laser beam 28 is a fixed value, the farther the distance between the low power ultraviolet microscope objective 8 and the long working distance high power ultraviolet microscope objective 25 is, the larger the diameter of the cone-shaped laser beam 28 is than the diameter of the entrance pupil 26, the weaker the laser energy passing through the long working distance high power ultraviolet microscope objective 25 is, but the smaller the focusing spot is; therefore, the distance between the low-power ultraviolet microscope objective 8 and the long-working distance high-power ultraviolet microscope objective 25 can be adjusted to make a trade-off between the laser energy passing through the long-working distance high-power ultraviolet microscope objective 25 and the focused light spot size, namely a large energy large light spot and a small energy small light spot; the echo signal reversely passes through the high-power ultraviolet microscope objective lens 25 with a long working distance along the main optical axis 4, and after being reflected by the dichroic mirror 27, the echo signal travels along the receiving optical axis 15, and then is split into two orthogonal paths after reaching the proportional beam splitter 17 (in this embodiment, a 9 to 1 proportional beam splitter, namely, a transmission 9 and a reflection 1): one path of the reflected light travels along the imaging optical axis 10, is focused between one time and two times of focal length of the imaging lens 32 in the electronic eyepiece 11 through the tube lens 33, and forms an amplified real image to the image sensor 31 through the imaging lens 32 (the embodiment adopts a black-and-white area array sensor, and the response wave band of the sensor is 350-800 nanometers); the other path passes through the proportional beam splitter 17, is subjected to Rayleigh scattering filtering by an ultraviolet Rayleigh filter 16 (the Rayleigh filter with the wavelength of 360nm in the embodiment), is focused to the incident end face of an optical fiber 13 by a microscope objective 14, and enters a spectrometer 12 (the detection spectrum range of the spectrometer is 360-750nm, the optical resolution is 0.1nm and the effective pixel number is 2000 points) for analysis; the low-power ultraviolet microscope objective 8 is arranged on the secondary linear electric platform 9 and can carry out one-dimensional precise translation along the main optical axis 4 under the drive of the secondary motor driver 6; the long working distance high power ultraviolet microscope objective 25 is arranged on the main linear electric platform 22 and can carry out one-dimensional precise translation along the main optical axis 4 under the drive of the main motor driver 21; the translation of the secondary linear electric platform 9 is mainly used for changing the distance between the low-power ultraviolet microscope objective 8 and the long-working-distance high-power ultraviolet microscope objective 25; the translation of the main linear electric platform 22 is mainly used for accurately focusing the long working distance high power ultraviolet microscope objective lens 25; the main optical axis 4, the imaging optical axis 10 and the receiving optical axis 15 are coplanar; the main optical axis 4 is parallel to the imaging optical axis 10 and perpendicular to the receiving optical axis 15;
the optical head 2 is arranged on a three-dimensional precise electric platform 29, and the three-dimensional precise electric platform 29 can perform submicron-level three-dimensional precise movement under the drive of the three-dimensional motor driver 1;
the main controller 7 can send control instructions to the three-dimensional motor driver 1, the main motor driver 21, the secondary motor driver 6, the ultraviolet Raman laser 3, the image sensor 31 and the spectrometer 12; and can receive the output digital image of the image sensor 31 and the output spectral information of the spectrometer 12;
the self-adaptive Raman fluorescence imaging combined method provided by the invention comprises the following steps:
(1) Adaptive focal spot calibration for an intended focal spot
In the in-situ detection of deep space substances, raman focal points with different dimensions, i.e. expected focal spots 19, are required for different detection objects 23, for example, for minerals with a more uniform distribution, slightly larger-sized expected focal spots 19 may be used; whereas for more varying minerals, an expected focal spot 19 of very small size may be employed to achieve very fine micro-zone analysis;
first, for the basic properties of the detection object 23 according to the test area, the diameter of the intended focal spot 19 is set (in this embodiment, for olive Dan Kuangwu, the diameter of the intended focal spot 19 is set to 1.7 microns); placing the measurement reticle 24 in a test area under a long working distance high power ultraviolet microscope objective 25; the measurement reticle 24 has uniform scribe lines 20 thereon (the scribe line pitch of the measurement reticle used in this example is 10 microns);
the main controller 7 controls the ultraviolet Raman laser 3 to be started, and ultraviolet laser beams emitted by the ultraviolet Raman laser sequentially pass through the ultraviolet interference filter 5, the low-power ultraviolet microscope objective 8 and the bicolor mirror 27, and then are illuminated and focused to the measurement reticle 24 through the long-working-distance high-power ultraviolet microscope objective 25 to form a real-time focal spot 18; the reflected light of the measuring reticle 24 passes through the long working distance high-power ultraviolet microscope objective lens 25 along the main optical axis 4 in the reverse direction, is reflected by the bicolor mirror 27, is reflected by the proportional beam splitter 17, is focused by the tube lens 33, and is subjected to real-time microscopic imaging by the imaging lens 32 to the image sensor 31;
the main controller 7 receives the microscopic digital image output by the image sensor 31 and performs real-time image processing; acquiring the excircle profile of the real-time focal spot 18 by adopting an edge extraction algorithm, thereby determining an imaging region of the real-time focal spot 18, and calculating the average gray value G of all pixels in the imaging region;
the main controller 7 sends out an instruction to the main motor driver 21 to drive the main linear electric platform 22 to move downwards by one step; the main controller 7 receives the microscopic digital image output by the image sensor 31, determines the imaging area of the real-time focal spot 18, calculates the average gray value G of all pixels in the imaging area, and compares whether the G value is increased or decreased: if the G value increases, it indicates that the downward movement is in a direction approaching the focus; if the G value decreases, it indicates that the upward movement is in a direction approaching the focus;
the main controller 7 sends out an instruction to the main motor driver 21 to drive the main linear electric platform 22 to move towards the direction approaching to the focus, and simultaneously calculates the average gray value G of all pixels in the imaging area of the real-time focal spot 18 in real time until the G value reaches the maximum value, and the main controller 7 sends out an instruction to the main motor driver 21 to stop moving in the tight focusing state;
in a tight focusing state, the main controller 7 acquires the linear position of the reticle 20 of the measurement reticle 24 and the outline of the outer circle of the real-time focal spot 18 by adopting an edge extraction algorithm on the microscopic digital image output by the image sensor 31, and then calculates the number of pixels at intervals of adjacent reticles 20 and the number of pixels of the diameter of the outline of the outer circle of the real-time focal spot 18, so that the diameter of the real-time focal spot 18 is calculated according to the distance between the reticles 20;
if the diameter of the real-time focal spot 18 is larger than the diameter of the expected focal spot 19, the main controller 7 sends a command to the secondary motor driver 6 to drive the secondary linear electric platform 9 to move upwards, the distance between the low-power ultraviolet microscope objective 8 and the long-power ultraviolet microscope objective 25 is increased, at the moment, the laser energy passing through the long-power ultraviolet microscope objective 25 is weakened, but the real-time focal spot 18 is reduced until the diameter of the real-time focal spot 18 is equal to the diameter of the expected focal spot 19, and the main controller 7 sends a command to the secondary motor driver 6 to stop the movement of the secondary linear electric platform 9;
similarly, if the diameter of the real-time focal spot 18 is smaller than the diameter of the expected focal spot 19, the main controller 7 sends a command to the secondary motor driver 6 to drive the secondary linear electric platform 9 to move downwards, the distance between the low-power ultraviolet microscope objective 8 and the long-power ultraviolet microscope objective 25 is reduced, at this time, the laser energy passing through the long-power ultraviolet microscope objective 25 is increased, the real-time focal spot 18 is increased until the diameter of the real-time focal spot 18 is equal to the diameter of the expected focal spot 19, and the main controller 7 sends a command to the secondary motor driver 6 to stop the movement of the secondary linear electric platform 9;
(2) Single point tight focusing of detected object
Removing the measurement reticle 24, and moving the adaptive Raman fluorescence imaging combined system into an actual test area, wherein the detection object 23 is positioned below the optical head 2, and the distance from the long working distance high-power ultraviolet microscope objective lens 25 is far greater than the focal length of the detection object;
the main controller 7 controls the ultraviolet Raman laser 3 to be started, ultraviolet laser beams emitted by the ultraviolet Raman laser sequentially pass through the ultraviolet interference filter 5, the low-power ultraviolet microscope objective 8 and the bicolor mirror 27, then defocused to the surface of the detection object 23 through the long-working-distance high-power ultraviolet microscope objective 25, reflected light passes through the long-working-distance high-power ultraviolet microscope objective 25 along the main optical axis 4 in the reverse direction, is reflected by the bicolor mirror 27, is reflected by the proportional beam splitter 17, is focused through the tube lens 33, and is microimaged to the image sensor 31 in real time through the imaging lens 32; the main controller 7 receives the microscopic digital image output by the image sensor 31 and performs fast fourier transformation to extract the high frequency component H thereof;
the main controller 7 sends out instructions to the three-dimensional motor driver 1 to drive the optical head 2 on the three-dimensional precise electric platform 29 to move downwards along the Z axis, at this time, the distance between the detected object 23 and the long working distance high-power ultraviolet microscope objective 25 is reduced, during the movement, the main controller 7 continuously carries out fast Fourier transform on the microscopic digital image output by the image sensor 31 in real time, and continuously extracts the high-frequency component H until the H reaches the maximum value, at this time, the laser is tightly focused to a point on the surface of the detected object 23, the size of the real-time focal spot 18 is equal to the size of the expected focal spot 19, and at this time, the laser is in a tightly focused state;
(3) Raman fluorescence and imaging information acquisition
In this tight focusing state, the main controller 7 records the three-dimensional displacement amount of the three-dimensional precision motorized stage 29, and sets it as the initial three-dimensional coordinate (x 1 ,y 1 ,z 1 ) The method comprises the steps of carrying out a first treatment on the surface of the The main controller 7 receives the microscopic digital image output by the image sensor 31, acquires the outline of the outer circle of the real-time focal spot 18 by adopting an edge extraction algorithm, thereby determining the imaging area of the real-time focal spot 18, and calculating the average gray value g of all pixels in the imaging area 1 The method comprises the steps of carrying out a first treatment on the surface of the The Raman and fluorescence backscattering of the real-time focal spot 18 position on the surface of the detection object 23 passes through the long working distance high-power ultraviolet microscope objective lens 25 along the main optical axis 4, is reflected by the bicolor lens 27, passes through the proportional beam splitter 17, filters the Rayleigh scattering of the wavelength of the ultraviolet Raman laser 3 by the ultraviolet Rayleigh filter 16, is focused to the incident end face of the optical fiber 13 by the microscope objective lens 14, enters the spectrometer 12, and the spectrometer 12 transmits the spectrum informationThe number is output to the main controller 7 for analysis; the main controller 7 first extracts n (in this embodiment n=3) discrete raman lines λ of the spectral signal 1 ，λ 2 ，λ 3 ，...，λ n Record the spectral line intensity I 11 ，Ι 12 ，Ι 13 ，...，Ι 1n The method comprises the steps of carrying out a first treatment on the surface of the The continuous fluorescence line is then divided into m segments of equal spectral interval (m=300 in this example); and recording the average intensity J of the fluorescence spectrum of each segment 11 ，J 12 ，J 13 ，...，J 1m ；
(4) Scanning micro-area analysis
The main controller 7 determines the number of scanning points A, B in the XY direction of the micro-area analysis, and the scanning step C, D; the main controller 7 sends an instruction to the three-dimensional motor driver 1 to drive the optical head 2 on the three-dimensional precise electric platform 29 to perform S-shaped scanning of an XY plane (namely, after scanning along an X axis to A points according to a scanning step length C, the Y axis moves forward by a step length D, then the Y axis moves reversely by a step length D, then the Y axis moves forward by A points, then the X axis moves reversely by a step length D, then the X axis moves reversely by A points, the number of common scanning points is A multiplied by B, namely A is multiplied by B), and each point on the XY plane moves up and down along a Z axis, so that single-point tight focusing of the step (2) is executed;
for each scanning point i (i is equal to or greater than 2 until i is equal to a×b), in the tightly focused state of the point, the main controller 7 records the three-dimensional displacement amount of the three-dimensional precision electric stage 29, determines the three-dimensional coordinates (x i ,y i ,z i ) The method comprises the steps of carrying out a first treatment on the surface of the The main controller 7 receives the microscopic digital image output by the image sensor 31, acquires the outline of the outer circle of the real-time focal spot 18 by adopting an edge extraction algorithm, thereby determining the imaging area of the real-time focal spot 18, and calculating the average gray value g of all pixels in the imaging area i The method comprises the steps of carrying out a first treatment on the surface of the The main controller 7 records n discrete Raman spectral lines lambda 1 ，λ 2 ，λ 3 ，...，λ n Line intensity I) i1 ，Ι i2 ，Ι i3 ，...，Ι in The method comprises the steps of carrying out a first treatment on the surface of the And recording the average intensity J of the fluorescence spectrum of each section of the m sections of the fluorescence spectrum i1 ,J i2 ,J i3 ,...,J im ；
The main controller 7 firstly synthesizes three-dimensional coordinates of A multiplied by B scanning points and draws the three-dimensional geometric morphology of the surface of the detection object 23 of the scanning area; then, g of each scanning point is integrated 1 ,g 2 ,...,g i ,., a grey-scale image of the three-dimensional geometry of the surface of the test object 23 can be obtained (this example is a broad spectrum image with a response band of 350 to 800 nm); then, the I of each scanning point is integrated 11 ,I 21 ,...,I i1 ,., the wavelength of the surface of the object to be inspected 23 is lambda 1 Similarly, the I of each scanning point is integrated 12 ,I 22 ,...,I i2 ,., the wavelength of the surface of the object to be inspected 23 is lambda 2 Until the wavelength of the surface of the detection object 23 is found to be λ n Raman image of (a); finally, integrating J of each scanning point 11 ,J 21 ,...,J i1 ,., obtaining a fluorescence image of a first spectral band of the surface of the object 23, and similarly integrating the J of the individual scan points 12 ,J 22 ,...,J i2 ,., obtaining a fluorescence image of a second spectral band of the surface of the object of detection 23, until a fluorescence image of an m-th spectral band of the surface of the object of detection 23 is obtained;
thus, the micro-region analysis is completed, and three-dimensional morphology distribution of the micro-region, and wide-spectrum images of A multiplied by B scanning points, ultraviolet laser Raman images of n wavelengths and ultraviolet laser-induced fluorescence hyperspectral images of m spectral bands on the three-dimensional morphology distribution are obtained.
Claims (1)
1. A deep space detection micro-area self-adaptive Raman fluorescence imaging combined system comprises a main controller (7), a spectrometer (12), an optical fiber (13), a three-dimensional motor driver (1), a three-dimensional precise electric platform (29) and an optical head (2); the method is characterized in that:
the optical head (2) consists of an ultraviolet Raman laser (3), an ultraviolet interference filter (5), a secondary motor driver (6), a secondary linear electric platform (9), a low-power ultraviolet microscope objective (8), a bicolor mirror (27), a long-working-distance high-power ultraviolet microscope objective (25), a main motor driver (21), a main linear electric platform (22), an ultraviolet Rayleigh filter (16), a proportional beam splitter (17), a microscope objective (14), a tube lens (33) and an electronic eyepiece (11); an imaging lens (32) and an image sensor (31) are arranged in the electronic eyepiece (11);
the cylindrical near-collimation laser beam (30) emitted by the ultraviolet Raman laser (3) along the main optical axis (4) passes through the ultraviolet interference filter (5) and can filter out the frequency division harmonic interference of the ultraviolet laser emitted by the ultraviolet Raman laser (3), so that the signal-to-noise ratio of the excited Raman signal is higher; the cylindrical near-collimation laser beam (30) passes through the ultraviolet interference filter (5) and then passes through the low-power ultraviolet microscope objective (8) to form a conical laser beam (28); after passing through the dichroic mirror (27), the cone-shaped laser beam (28) reaches the entrance pupil (26) of the long working distance high-power ultraviolet microscope objective (25), at the position of the entrance pupil (26), the diameter of the cone-shaped laser beam (28) is larger than that of the entrance pupil (26), and as the cone angle of the cone-shaped laser beam (28) is a fixed value, the distance between the low-power ultraviolet microscope objective (8) and the long working distance high-power ultraviolet microscope objective (25) is longer, the diameter of the cone-shaped laser beam (28) is larger than that of the entrance pupil (26), the laser energy passing through the long working distance high-power ultraviolet microscope objective (25) is weaker, but the focusing light spot is smaller; therefore, the distance between the low-power ultraviolet microscope objective lens (8) and the long-working distance high-power ultraviolet microscope objective lens (25) can be adjusted to make a trade-off between the laser energy passing through the long-working distance high-power ultraviolet microscope objective lens (25) and the focused light spot size, namely a large energy large light spot and a small energy small light spot; the echo signal reversely passes through the high-power ultraviolet microscope objective lens (25) with a long working distance along the main optical axis (4), and the double-color lens (27) moves along the receiving optical axis (15) after being reflected, and is divided into two orthogonal paths after reaching the proportional beam splitter (17): one path of reflected light travels along an imaging optical axis (10), is focused between one time and two times of focal length of an imaging lens (32) in an electronic eyepiece (11) through a tube lens (33), and forms an amplified real image to an image sensor (31) through the imaging lens (32); the other path passes through a proportional beam splitter (17), is subjected to Rayleigh scattering filtering of the wavelength of an ultraviolet Raman laser (3) through an ultraviolet Rayleigh filter (16), is focused to the incident end face of an optical fiber (13) through a microscope objective (14), and then enters a spectrometer (12) for analysis; the low-power ultraviolet microscope objective (8) is arranged on the secondary linear electric platform (9) and can carry out one-dimensional precise translation along the main optical axis (4) under the drive of the secondary motor driver (6); the long working distance high power ultraviolet microscope objective (25) is arranged on the main linear electric platform (22) and can carry out one-dimensional precise translation along the main optical axis (4) under the drive of the main motor driver (21); the translation of the secondary linear electric platform (9) is mainly used for changing the distance between the low-power ultraviolet microscope objective (8) and the long-working-distance high-power ultraviolet microscope objective (25); the translation of the main linear electric platform (22) is mainly used for accurately focusing the high-power ultraviolet microscope objective lens (25) with a long working distance; the main optical axis (4), the imaging optical axis (10) and the receiving optical axis (15) are coplanar; the main optical axis (4) is parallel to the imaging optical axis (10) and perpendicular to the receiving optical axis (15);
the optical head (2) is arranged on a three-dimensional precise electric platform (29), and the three-dimensional precise electric platform (29) can perform submicron-level three-dimensional precise movement under the drive of a three-dimensional motor driver (1);
the main controller (7) can send control instructions to the three-dimensional motor driver (1), the main motor driver (21), the secondary motor driver (6), the ultraviolet Raman laser (3), the image sensor (31) and the spectrometer (12); and can receive the output digital image of the image sensor (31) and the output spectral information of the spectrometer (12).
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| CN107907526B (en) * | 2017-10-13 | 2023-09-12 | 中国科学院上海技术物理研究所 | Deep space detection micro-region self-adaptive Raman fluorescence imaging combined system |
| CN109239053B (en) * | 2018-10-29 | 2020-08-07 | 中国科学院上海技术物理研究所 | Astronaut urine detection system based on liquid core waveguide Raman spectrum |
| CN109358035B (en) * | 2018-10-29 | 2021-01-01 | 中国科学院上海技术物理研究所 | System for detecting transition metal in urine of astronaut in microgravity environment of space station |
| CN109342339B (en) * | 2018-10-29 | 2021-02-12 | 中国科学院上海技术物理研究所 | Micro-area map integrated detection system for environmental agriculture, forestry, animal and plant risk factors |
| CN109239052B (en) * | 2018-10-29 | 2020-10-16 | 中国科学院上海技术物理研究所 | Astronaut urine detection method based on liquid core waveguide Raman spectrum |
| CN109358034B (en) * | 2018-10-29 | 2020-08-07 | 中国科学院上海技术物理研究所 | Astronaut urine detection method based on liquid core waveguide combined spectrum |
| CN110530846A (en) * | 2019-09-19 | 2019-12-03 | 北京华泰诺安探测技术有限公司 | A kind of laser Raman spectroscopy detection system and its detection method |
| CN111521599B (en) * | 2020-06-15 | 2021-05-28 | 中国海洋大学 | Rapid detection system and method for micro-plastic in offshore sediments |
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