CN114076590A - Water area up-conversion fluorescence vortex detection device and detection method thereof - Google Patents

Water area up-conversion fluorescence vortex detection device and detection method thereof Download PDF

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CN114076590A
CN114076590A CN202111494038.5A CN202111494038A CN114076590A CN 114076590 A CN114076590 A CN 114076590A CN 202111494038 A CN202111494038 A CN 202111494038A CN 114076590 A CN114076590 A CN 114076590A
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image
image acquisition
storage bin
aircraft
processing system
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付姚
胡雅茜
温永盛
曾瑞浪
李竖斌
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Dalian Maritime University
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Dalian Maritime University
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01C—MEASURING DISTANCES, LEVELS OR BEARINGS; SURVEYING; NAVIGATION; GYROSCOPIC INSTRUMENTS; PHOTOGRAMMETRY OR VIDEOGRAMMETRY
    • G01C13/00—Surveying specially adapted to open water, e.g. sea, lake, river or canal
    • G01C13/002—Measuring the movement of open water
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A90/00—Technologies having an indirect contribution to adaptation to climate change
    • Y02A90/30—Assessment of water resources

Abstract

The invention provides a water area up-conversion fluorescence vortex detection device and a detection method thereof, wherein the device comprises a shell, a laser emitter, a nanoparticle storage bin and an image acquisition and processing system, wherein the laser emitter emits infrared laser to a detection direction to irradiate; the nano-particle storage bin emits a bullet filled with hydrophilic upconversion nano-powder to the direction to be detected, the bullet is blasted in a designated area, and upconversion nano-particles are released; the up-conversion nano particles emit visible light under the excitation of infrared laser beams to present optical images; the image acquisition and processing system acquires optical images, and the optical images are processed to judge the turbulence condition of the water area. The invention can achieve the effects of signal transmitting-receiving device integration and underwater turbulence visualization, is beneficial to improving the accuracy and sensitivity of turbulence visualization imaging and enhancing the detectability of vortexes.

Description

Water area up-conversion fluorescence vortex detection device and detection method thereof
Technical Field
The invention relates to the technical field of water turbulence detection, in particular to a water up-conversion fluorescence vortex detection device and a detection method thereof.
Background
The turbulence is a special area with local non-uniform distribution of seawater density and concentration commonly existing in ocean lakes, and the scale of the turbulence is widely distributed from millimeter magnitude to tens of kilometers magnitude. The change of the ocean turbulence in a small range and a short time is rapid and random, and for a non-dragging aircraft, once the non-dragging aircraft encounters a torrent environment, the non-dragging aircraft is easy to be damaged by violent collision with hard objects such as an underwater reef. Therefore, detection of water area turbulence is achieved, and the method has great significance for adjusting the advancing course in time and improving the navigation safety and stability of the underwater vehicle, particularly the non-dragging intelligent underwater vehicle.
At present, the detection of the water area environment target is mainly realized by ultra-long wave detection and sound wave detection. However, the ultra-long wave detection system has the disadvantages of complexity, large power consumption, narrow pass band and the like, and the disadvantages of low sound wave transmission speed, long delay, serious doppler dispersion, poor security and the like are also inevitable. Under the background, the underwater optical detection mode provides a new idea for the detection technology. At present, the research aiming at the underwater turbulence optical detection is mainly vortex beam detection and particle imaging technology. Through analysis, the common problem of the foregoing optical detection methods is that the emitting device of the detection signal and the receiving device of the feedback signal must be distributed in different directions of the detected area, and cannot be installed on the same carrier (e.g., an aircraft), and therefore, the optical detection methods cannot be applied to an aircraft body and complete real-time autonomous detection and risk avoidance. In addition, in the existing optical detection process, optical accessories such as a reflector and the like are required to change the propagation direction of the light beam for many times, and the required equipment is large in size and low in detection sensitivity.
Disclosure of Invention
According to the defects of complex system, large power consumption, narrow passband and the like in the superlong wave detection, the defects of low transmission speed, long delay, serious Doppler frequency dispersion, poor confidentiality and the like in the sound wave detection, and the technical problems of huge equipment volume, different real-time signal transmission and information receiving and different bodies in the water turbulence detection of an optical detection method, the device for detecting the converted fluorescence vortex on the water and the detection method thereof are provided. The invention mainly realizes 'turbulent flow visualization' by exciting up-conversion luminescent particles by an infrared laser, and carries out image acquisition and comparative analysis on the water self-luminous optical image.
The technical means adopted by the invention are as follows:
a fluorescence vortex detection device in water, mounted on an aircraft, comprising: the device comprises a shell, a laser emitter, a nanoparticle storage bin and an image acquisition and processing system, wherein the laser emitter, the nanoparticle storage bin and the image acquisition and processing system are packaged in the shell and are sequentially arranged from top to bottom;
the laser emitter and the nanoparticle storage bin are both connected with an image acquisition and processing system, and the laser emitter is used for emitting infrared laser to the direction to be detected for irradiation; the nanoparticle storage bin is used for emitting a projectile filled with hydrophilic upconversion nano powder to a detection direction, the projectile is exploded in a designated area to release upconversion nanoparticles, the upconversion nanoparticles are positioned in an irradiation range of infrared laser, and the upconversion nanoparticles emit visible light and present an optical image under the excitation of infrared laser beams; the image acquisition and processing system is used for acquiring optical image data, and judging the turbulence condition of a water area through processing and displaying;
the image acquisition processing system comprises an image acquisition module, an image processing module and an image display module, wherein the image acquisition module is simultaneously connected with the laser emitter and the nanoparticle storage bin and is used for acquiring optical image data; the image processing module is respectively connected with the image acquisition module and the image display module through network cables and is used for receiving the original optical image data acquired by the image acquisition module, carrying out image enhancement processing on the original optical image data and transmitting the processed image to the image display module for display.
Further, the nanoparticle storage bin is disposed 1cm from the top of the housing.
Further, the laser emitter is arranged 1.5cm under the nanoparticle storage bin, emits infrared laser at a depression angle of 5 degrees, and expands the beam through the arranged beam expander.
Further, the image acquisition processing system is arranged at a position 2cm below the laser transmitter, and the distance between the image acquisition processing system and the bottom of the shell is 1 cm.
Furthermore, the image acquisition and processing system adopts an integrated hardware acquisition and processing design scheme, the image acquisition and processing tasks are realized by the same hardware board card, the data exchange between the two is realized by an on-board bus (or other data communication modes such as FIFO (first in first out), double RAM (random access memory) alternation and the like), the image acquisition is completed by a special digital conversion module, the image processing is realized by a special DSP (or DSP array) module, and the modules adopt a tight coupling integrated design.
The invention also provides a detection method of the device for detecting the converted fluorescence vortex in the water area, which comprises the following steps:
firstly, a laser emitter carried by an aircraft emits infrared laser at a depression angle of 5 degrees to a direction to be detected for irradiation;
step two, at the same time, a nanoparticle storage bin of the aircraft emits a projectile filled with hydrophilic upconversion nano powder to the direction to be detected, the projectile is exploded in a designated area, and upconversion nanoparticles are released;
thirdly, emitting visible light by the up-conversion nano particles under the excitation of the infrared laser beam to present an optical image;
fourthly, an image acquisition and processing system carried by the aircraft acquires optical images, and the optical images are processed to judge the turbulence condition of the water area; after the laser emitter and the nanoparticle storage bin emit laser searchlighting and up-conversion nano powder projectiles at the same time, the image acquisition module is triggered to acquire optical image data, the optical image data are transmitted to the image processing module, and the image processing module transmits the optical image data to the image display module for displaying after image enhancement processing is carried out on the optical image data.
Further, in the first step, a method for irradiating the laser emitter carried by the aircraft by emitting infrared laser to the direction to be detected includes: when the aircraft moves to an unknown water area, a laser emitter carried by the aircraft emits 808nm infrared laser at a depression angle of 5 degrees to the direction to be detected, and the infrared laser irradiates forwards after beam expansion.
Further, in the second step, the nanoparticle storage bin of the aircraft emits a projectile loaded with hydrophilic upconversion nanopowder in the direction to be detected, and the method for releasing upconversion nanoparticles by blasting the projectile in the designated area includes: launching a bullet filled with hydrophilic upconversion nano powder from a nano particle storage bin of an aircraft to a direction to be detected, blasting the bullet in a designated area, releasing the upconversion nano particles, and rapidly diffusing in the designated area to form sol;
the up-conversion nano powder comprises but is not limited to NaYF4:Nd3+,Yb3+,Er3+@NaYF4:Nd3+@SiO2、NaGdF4:Yb3+,Er3+@NaGdF4@PDAs、BaGdF4:Yb3+,Er3+、NaYF4:Yb3+,Er3+@NaYF4:Yb3+,Nd3+@PDAs、NaYbF4:Er3+@NaYbF4:Tm3+@NaYF4、NaYF4:Yb3+,Tm3+@CaF2、NaYF4:Yb3+,Tm3+,Ce3+、NaLuF4:Yb3+,Tm3+,Er3+、NaLuF4:Yb3+,Tm3+Or Gd2O3:Yb3+,Ho3+And the like.
Further, in the third step, the upconversion nanoparticles emit visible light under excitation of the infrared laser beam, and the method for presenting an optical image includes: the up-conversion nano particles emit different color lights under the excitation of 808nm infrared laser beams, and the modulation of different color lights and different luminous intensities in a visible light range can be realized by adjusting the doping ion species and the doping concentration ratio of the up-conversion nano powder; the vortex structure generated by the turbulence effect carries the up-conversion nano particles to form random spatial distribution, and a stable distribution state can be formed in a still water environment, so that the distribution state of the nano colloid particles can present a static or dynamic optical image to reflect the water vortex structure.
Further, in the fourth step, the method for determining the turbulence of the water area by processing the optical image acquired by the image acquisition and processing system carried by the aircraft includes: the optical image is a self-luminous phenomenon, the image acquisition module carried by an aircraft acquires the optical image of the nano colloidal particles in the unknown water area state, the image processing module performs enhancement processing on the optical image by using a soluble operator based on the motion compensation principle, and the optical image distribution condition of the still water environment in an image database is compared after the optical image is displayed by the image display module to judge the turbulence degree of the water body.
Compared with the prior art, the invention has the following advantages:
1. the invention provides a water area up-conversion fluorescence vortex detection device and a detection method thereof, which can achieve the purposes of integration of a signal transmitting-receiving device and visualization of underwater turbulence by collecting, processing and analyzing specific self-luminous images of up-conversion nano particles presented along with vortex water flow, and solve the problems that the signal transmitting and receiving devices of a detection system are different and feedback signals are difficult to transmit to a navigation equipment body in the prior art.
2. According to the water area up-conversion fluorescence vortex detection device and the detection method thereof, the hydrophilic up-conversion nano particles are used as the luminescent material, and the accuracy and the sensitivity of turbulent flow visualization imaging are improved by utilizing the good monodispersity of the hydrophilic up-conversion nano particles in the water.
3. The water area up-conversion fluorescence vortex detection device and the detection method thereof provided by the invention comprehensively consider the absorption spectrum of water, and reduce the light-emitting loss to the maximum extent by selecting the combined up-conversion luminescence mechanism of '808 nm excitation-550 nm emission', thereby being beneficial to improving the stability of the underwater optical detection technology and enhancing the detectability.
In conclusion, the technical scheme of the invention can solve the problems that the signal transmitting and receiving devices of the detection system are different, the feedback signals are difficult to transmit to the navigation equipment body, the detection equipment is large in size, the detection means is complex and the detection sensitivity is low in the existing underwater optical detection technology.
Based on the reasons, the invention can be widely popularized in the fields of ships, water area aircrafts and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a diagram of an integrated vortex detection device of the present invention.
FIG. 2 is a schematic flow chart of the detection method of the present invention.
Figure 3 is a TEM image of a core nanoparticle of the present invention.
FIG. 4 is a TEM image of a core-shell nanoparticle of the present invention.
FIG. 5 is a luminescence intensity spectrum of the core-shell nanoparticle of the present invention.
Fig. 6 is a diagram of the energy levels of the core-shell nanoparticles of the present invention.
Fig. 7 is a TEM image of the core-shell nanoparticles of the present invention after hydrophilic modification.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective portions shown in the drawings are not drawn in an actual proportional relationship for the convenience of description. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. Any specific values in all examples shown and discussed herein are to be construed as exemplary only and not as limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.
Example 1
As shown in fig. 1, the present invention provides a fluorescence vortex detection device converted in water, which is based on the principle of up-conversion luminescence and optics, and is installed on an aircraft, and includes a housing, a laser emitter, a nanoparticle storage bin, and an image acquisition and processing system. The image acquisition processing system comprises an image acquisition module, an image processing module and an image display module.
The laser transmitter is connected with the image acquisition module and emits infrared laser to the direction to be detected for irradiation.
The nano-particle storage bin is connected with the image acquisition module, and is used for launching the projectile filled with the hydrophilic upconversion nano-powder to the detection direction, and the projectile is exploded in the designated area to release upconversion nano-particles.
After the laser emitter and the nanoparticle storage bin simultaneously emit laser searchlighting and the upconversion nano powder projectile, the image acquisition module is triggered to acquire optical image data presented by visible light emitted by the upconversion nanoparticles under the excitation of the infrared laser beam.
One end of the image processing module is connected with the image acquisition module through a network cable and is used for receiving original optical image data and carrying out image enhancement processing on the original optical image data; the other end is connected with the image display module, and the processed image is transmitted to the image display module to be displayed.
The installation positions of the image acquisition and processing system, the laser emitter and the nanoparticle storage bin are as follows:
the nano particle storage bin, the laser emitter and the image acquisition processing system are packaged in the same shell to form an integrated vortex detection device, and the nano particle storage bin, the laser emitter and the image acquisition processing system are sequentially arranged on the same vertical line from top to bottom. The specific location information and design factors are as follows:
considering that the up-conversion nano powder particles are influenced by gravity in the water area environment and the action that local aggregation may occur under the internal vortex action of fluid exists, the nano particle storage bin is arranged at the uppermost part and is 1cm away from the top of the upper shell of the shell. And a 808nm laser transmitter is arranged at a position 1.5cm under the nanoparticle storage bin, emits infrared laser at a depression angle of 5 degrees, and expands the beam through a beam expander. Considering that the high power of the emergent laser possibly causes certain influence on the image acquisition processing system, the image acquisition processing system is arranged 2cm under the laser transmitter to acquire data of self-luminous imaging of the upper-mounted and replaceable nano particles under infrared irradiation, and the distance between the image acquisition processing system and the bottom of the lower shell of the shell is 1 cm.
Example 2
As shown in fig. 2, on the basis of embodiment 1, the present invention provides a detection method of a fluorescence vortex detection device converted on a water area, which comprises the following steps performed in sequence:
1) and a laser emitter carried by the aircraft emits infrared laser to the direction to be detected for irradiation.
2) A bullet cabin (nanoparticle storage cabin) arranged in the aircraft emits a bullet filled with hydrophilic upconversion nano powder to a detection direction, and the bullet explodes in a designated area to release upconversion nanoparticles.
3) The up-conversion nano particles emit visible light under the excitation of the infrared laser beam to present an optical image.
4) An image acquisition and processing system carried by the aircraft acquires optical images, and the optical images are processed to judge the turbulence condition of the water area.
In the present embodiment, the method for irradiating the laser beam emitted in the direction to be detected by the laser emitter mounted on the aircraft in step 1) includes: when the aircraft moves to an unknown water area, a laser emitter carried by the aircraft emits 808nm infrared laser to a direction to be detected, and the infrared laser irradiates forwards after beam expansion.
In this embodiment, the method for launching the projectile loaded with the hydrophilic upconversion nano powder to the detection direction by the internal magazine of the aircraft in the step 2), wherein the method for releasing the upconversion nano particles by the projectile is as follows: and launching the projectile filled with the hydrophilic upconversion nano powder to the direction to be detected by the built-in magazine of the aircraft, wherein the projectile is exploded in a designated area to release upconversion nano particles and quickly diffuse in the designated area to form sol. The upconversion nanopowder includes but is not limited to NaYF4:Nd3+,Yb3+,Er3+@NaYF4:Nd3+@SiO2、NaGdF4:Yb3+,Er3+@NaGdF4@PDAs、BaGdF4:Yb3+,Er3+、NaYF4:Yb3+,Er3+@NaYF4:Yb3+,Nd3+@PDAs、NaYbF4:Er3+@NaYbF4:Tm3+@NaYF4、NaYF4:Yb3+,Tm3+@CaF2、NaYF4:Yb3+,Tm3+,Ce3+、NaLuF4:Yb3+,Tm3+,Er3+、NaLuF4:Yb3+,Tm3+Or Gd2O3:Yb3+,Ho3+And the like. In this embodiment, a hydrophilic upconversion nano-powder NaYF is selected4:Nd3+,Yb3+,Er3+@NaYF4:Nd3+@SiO2。
In this embodiment, the method for emitting visible light by the upconversion nanoparticles in step 3) under the excitation of the infrared laser beam to present an optical image includes: the up-conversion nano particle NaYF4:Nd3+,Yb3+,Er3+@NaYF4:Nd3+@SiO2Under the excitation of a laser beam with 808nm, bright green light and relatively weaker red light are emitted, and the branch ratio of the green light to the red light reaches 8.25. The vortex structure generated by the turbulence effect carries the up-conversion nano particles to form random spatial distribution, and a stable distribution state can be formed in a still water environment, so that the distribution state of the nano colloid particles can present a static or dynamic optical image to reflect the water vortex structure.
In this embodiment, the method for determining the turbulence in the water area by acquiring an optical image with the image acquisition and processing system carried by the aircraft in step 4) and processing the optical image includes: the optical image is a self-luminous phenomenon, the image acquisition module carried by the aircraft acquires the optical image of the nano colloidal particles of unknown water area conditions, the image processing module performs enhancement processing on the optical image by using a soluble operator based on a motion compensation principle, and the optical image distribution condition of the still water environment in the image database is compared after the optical image is displayed by the image display module to judge the turbulence degree of the water body.
According to the invention, the specific self-luminous image presented by the up-conversion nano particles along with the vortex water flow is collected, processed and analyzed, so that the purposes of integration of the signal transmitting-receiving device and visualization of underwater turbulence can be achieved, and the problems that different bodies of the signal transmitting and receiving device of the detection system and feedback signals are difficult to transmit to the navigation equipment body in the prior art are solved.
The invention adopts hydrophilic NaYF4:Nd3+,Yb3+,Er3+@NaYF4:Nd3+@SiO2The up-conversion nanoparticles are used as a luminescent material, and the accuracy and the sensitivity of turbulent flow visual imaging are improved by utilizing the good monodispersity of the up-conversion nanoparticles in a water body.
The invention comprehensively considers the absorption spectrum of water, and reduces the light-emitting loss to the maximum extent by selecting a combined up-conversion light-emitting mechanism of '808 nm excitation-550 nm emission', thereby being beneficial to improving the stability of the underwater optical detection technology and enhancing the detectability thereof.
Example 3
On the basis of embodiment 2, the invention also provides a hydrophilic Nd3+The preparation method of the sensitized nano particle adopts a high-temperature coprecipitation method to prepare monodisperse lanthanide ion doped NaYF4Up-converting the core nanoparticle. Then, the surface of the nuclear nano particle is coated with NaYF by adopting an epitaxial layer growth method4An inert shell layer. The preparation method comprises the following specific steps:
1) synthesis of NaYF4:Nd3+,Yb3+,Er3+Core nanoparticles
(1) At room temperature (23-25 deg.C), 3ml OA (oleic acid), 7ml ODE (1-octadecene), 2ml Ln (CH) were aspirated respectively by pipette3CO2)3(0.2M) aqueous solution to a 50ml two-necked flask (with addition of a pyromagnetite);
(2) placing the two-mouth flask in an oil bath pot, setting the temperature of a heating device to 130 ℃, after the water in the liquid in the two-mouth flask is completely evaporated, heating to 150 ℃, and keeping the temperature for 60 min;
(3) stopping heating, keeping the magnetons to continuously rotate, and slowly cooling the mixed solution to room temperature;
(4) moving the two bottles into a heating sleeve, and setting the temperature of the heating sleeve to keep the temperature of the solution at 50 ℃;
(5) pipette with 2ml NaOH (0.5M) and 4ml NH, respectively4F(0.4M) adding a methanol solution into a 15ml centrifuge tube, covering a cover tightly, quickly injecting into a two-neck flask after vortex oscillation, keeping the temperature at 50 ℃ for 30 min;
(6) adjusting the temperature of the heating jacket to 110 ℃ to remove methanol in the solution, and connecting the two-mouth flask with the double-row pipes after the methanol is removed;
(7) vacuumizing for 10min, and introducing N for a short time2Repeating the above steps for three times;
(8) adjusting the temperature of the heating jacket to heat the solution to 290 ℃ (heating rate 10 ℃/min), keeping the temperature for 1.5h, and slowly introducing N in the whole process2；
(9) Taking down the heating sleeve, keeping the magnetons to continue rotating, and naturally cooling the solution to room temperature;
(10) transferring the mixed solution to a 50ml centrifuge tube, adding 30ml ethanol, placing in a centrifuge, centrifuging at 8000rpm for 8min, and pouring off the supernatant;
(11) adding 4ml of cyclohexane into a centrifugal tube, adding 15ml of ethanol after ultrasonic dispersion, putting the mixture into a centrifugal machine, centrifuging the mixture at the rotating speed of 8000rpm for 8min, removing supernatant, and repeating the step twice;
(12) 4ml of cyclohexane was added to the centrifuge tube, and after ultrasonic dispersion the solution was transferred to a 5ml reagent bottle and labeled and stored in a refrigerator at 4 ℃ until use. TEM tests prove that the sample is monodisperse nanoparticles with the diameter of about 20nm, as shown in figure 3.
2) Synthesis of NaYF4:Nd3+,Yb3+,Er3+@NaYF4:Nd3+Core-shell nanoparticles
(1) At room temperature (23-25 deg.C), 3ml OA (oleic acid), 7ml ODE (1-octadecene), 2ml Ln (CH) were aspirated respectively by pipette3CO2)3(0.2M) aqueous solution to a 50ml two-necked flask (with addition of a pyromagnetite);
(2) placing the two-mouth flask in an oil bath pot, setting the temperature of a heating device to 130 ℃, after the water in the liquid in the two-mouth flask is completely evaporated, heating to 150 ℃, and keeping the temperature for 60 min;
(3) stopping heating, keeping the magnetons to continuously rotate, and slowly cooling the mixed solution to room temperature;
(4) moving the two bottles into a heating sleeve, and setting the temperature of the heating sleeve to keep the temperature of the solution at 50 ℃;
(5) pipette 4ml of NaYF solution separately with pipette4:Nd3+,Yb3+,Er3+Transferring the cyclohexane solution into a two-neck flask, and heating for 10 min;
(6) pipette with 2ml NaOH (0.5M) and 4ml NH, respectively4F (0.4M) methanol solution is put into a 15ml centrifuge tube, a cover is tightly covered, the mixture is quickly injected into a two-neck flask after vortex oscillation, and the constant temperature is kept at 50 ℃ for 30 min;
(7) the reaction process is the same as the processes (6) to (12) in section 1); TEM tests prove that the sample diameter is increased to about 25nm and still in a monodisperse state, which shows that the shell coating is successfully realized (see figure 4).
The nanoparticles were tested to exhibit bright green emission under excitation by an 808nm infrared laser, the emission spectrum of which is shown in fig. 5. It can be seen that the upconversion luminescence of the nanoparticles is composed of 520-560nm green light and relatively weaker 640-670nm red light emission, and the green-red branch ratio reaches 8.25. FIG. 6 is a transition energy level diagram of an Er-Yb-Nd-Nd system, which can be helpful for analyzing the up-conversion luminescence process of the nano-particles.
3) Synthesis of NaYF4:Nd3+,Yb3+,Er3+@NaYF4:Nd3+@SiO2Hydrophilically modified nanoparticles
(1) Taking NaYF4:Nd3+,Yb3+,Er3+@NaYF4:Nd3+(2ml,0.1M) was mixed with hydrochloric acid (2ml,2M), poured into a 50ml beaker and sealed, after sonication at room temperature for 1h, the reaction solution was transferred into a 50ml centrifuge tube, centrifuged at 10000rpm for 5min, the supernatant was removed, and the precipitate was dissolved in 2ml of water (concentration 0.1M).
(2) Taking NaYF4:Nd3+,Yb3+,Er3+@NaYF4:Nd3+(2ml,0.1M), 2.5ml CO-520 was added and stirred for 10 min. 0.45ml of ammonia (mass fraction 25-28%) was added, the vessel was sealed and sonicated for 5min, after which 0.2ml of Tetraethylorthosilicate (TEOS) was added. The vessel was again sealed and stirred at 600rpm for 48 h. After the reaction, 50ml of acetone was added thereto at room temperatureCentrifuging at 10000rpm for 5min, removing supernatant, washing nanoparticles with anhydrous ethanol and water (1:1) twice, precipitating with 50ml acetone, and centrifuging to obtain NaYF4:Nd3+,Yb3+,Er3+@NaYF4:Nd3+@SiO2Finally dissolved in 2ml of water (concentration 0.1M).
The TEM image of the modified core-shell nanoparticle is shown in FIG. 7, and SiO with a thickness of 10nm can be clearly seen on the surface of the upconversion nanoparticle2A thin layer. After modification, the nanoparticles can be well dispersed in water and do not aggregate and precipitate for a long time.
The invention can also be applied to the fields of ships, water area aircrafts and the like, and has potential application prospect and prominent practical significance for the fields of diving movement danger early warning and the like.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. A fluorescence vortex detection device in water, mounted on an aircraft, comprising: the device comprises a shell, a laser emitter, a nanoparticle storage bin and an image acquisition and processing system, wherein the laser emitter, the nanoparticle storage bin and the image acquisition and processing system are packaged in the shell and are sequentially arranged from top to bottom;
the laser emitter and the nanoparticle storage bin are both connected with an image acquisition and processing system, and the laser emitter is used for emitting infrared laser to the direction to be detected for irradiation; the nanoparticle storage bin is used for emitting a projectile filled with hydrophilic upconversion nano powder to a detection direction, the projectile is exploded in a designated area to release upconversion nanoparticles, the upconversion nanoparticles are positioned in an irradiation range of infrared laser, and the upconversion nanoparticles emit visible light and present an optical image under the excitation of infrared laser beams; the image acquisition and processing system is used for acquiring optical image data, and judging the turbulence condition of a water area through processing and displaying;
the image acquisition processing system comprises an image acquisition module, an image processing module and an image display module, wherein the image acquisition module is simultaneously connected with the laser emitter and the nanoparticle storage bin and is used for acquiring optical image data; the image processing module is respectively connected with the image acquisition module and the image display module through network cables and is used for receiving the original optical image data acquired by the image acquisition module, carrying out image enhancement processing on the original optical image data and transmitting the processed image to the image display module for display.
2. The apparatus of claim 1, wherein the nanoparticle storage bin is positioned 1cm from the top of the housing.
3. The apparatus of claim 1, wherein the laser emitter is disposed 1.5cm below the nanoparticle storage bin, emits infrared laser light at a depression angle of 5 °, and expands the beam via the beam expander.
4. The apparatus of claim 1, wherein the image acquisition and processing system is disposed 2cm directly below the laser transmitter and 1cm from the bottom of the housing.
5. The apparatus of claim 1, wherein the image acquisition and processing system is designed as an integrated hardware acquisition and processing system, the image acquisition and processing tasks are performed by the same hardware board, the data exchange between the hardware board and the hardware board is performed alternatively by an on-board bus, FIFO or dual RAM, the image acquisition is performed by a dedicated digital conversion module, the image processing is performed by a dedicated DSP or DSP array module, and the modules are designed as a tightly coupled module.
6. The method for detecting the fluorescence vortex detection device converted in the water area according to any one of the claims 1 to 5, comprising the following steps:
firstly, a laser emitter carried by an aircraft emits infrared laser at a depression angle of 5 degrees to a direction to be detected for irradiation;
step two, at the same time, a nanoparticle storage bin of the aircraft emits a projectile filled with hydrophilic upconversion nano powder to the direction to be detected, the projectile is exploded in a designated area, and upconversion nanoparticles are released;
thirdly, emitting visible light by the up-conversion nano particles under the excitation of the infrared laser beam to present an optical image;
fourthly, an image acquisition and processing system carried by the aircraft acquires optical images, and the optical images are processed to judge the turbulence condition of the water area; after the laser emitter and the nanoparticle storage bin emit laser searchlighting and up-conversion nano powder projectiles at the same time, the image acquisition module is triggered to acquire optical image data, the optical image data are transmitted to the image processing module, and the image processing module transmits the optical image data to the image display module for displaying after image enhancement processing is carried out on the optical image data.
7. The detection method of the fluorescence vortex detection device converted in water area according to claim 6, wherein in the first step, the method for irradiating the laser emitter carried by the aircraft to emit the infrared laser to the direction to be detected comprises: when the aircraft moves to an unknown water area, a laser emitter carried by the aircraft emits 808nm infrared laser at a depression angle of 5 degrees to the direction to be detected, and the infrared laser irradiates forwards after beam expansion.
8. The detection method of the fluorescence vortex detection device converted in water area as claimed in claim 6, wherein in the second step, the nanoparticle storage bin of the aircraft emits a projectile loaded with hydrophilic upconversion nanopowder in the direction to be detected, and the method for releasing upconversion nanoparticles by blasting the projectile in the designated area comprises: launching a bullet filled with hydrophilic upconversion nano powder from a nano particle storage bin of an aircraft to a direction to be detected, blasting the bullet in a designated area, releasing the upconversion nano particles, and rapidly diffusing in the designated area to form sol;
the up-conversion nano powder is NaYF4:Nd3+,Yb3+,Er3+@NaYF4:Nd3+@SiO2、NaGdF4:Yb3+,Er3+@NaGdF4@PDAs、BaGdF4:Yb3+,Er3+、NaYF4:Yb3+,Er3+@NaYF4:Yb3+,Nd3+@PDAs、NaYbF4:Er3+@NaYbF4:Tm3+@NaYF4、NaYF4:Yb3+,Tm3+@CaF2、NaYF4:Yb3+,Tm3+,Ce3+、NaLuF4:Yb3+,Tm3+,Er3+、NaLuF4:Yb3+,Tm3+Or Gd2O3:Yb3+,Ho3+。
9. The detection method of the vortex detection device with converted fluorescence in water area of claim 6, wherein in step three, the upconversion nanoparticles emit visible light under the excitation of infrared laser beam, and the method for presenting optical image is as follows: the up-conversion nano particles emit different color lights under the excitation of 808nm infrared laser beams, and the modulation of different color lights and different luminous intensities in a visible light range can be realized by adjusting the doping ion species and the doping concentration ratio of the up-conversion nano powder; the vortex structure generated by the turbulence effect carries the up-conversion nano particles to form random spatial distribution, and a stable distribution state can be formed in a still water environment, so that the distribution state of the nano colloid particles can present a static or dynamic optical image to reflect the water vortex structure.
10. The method for detecting the converted fluorescent vortex detection device in water area of claim 6, wherein in the fourth step, the image collecting and processing system carried by the aircraft collects the optical images, and the method for determining the turbulence condition of the water area after the optical images are processed comprises the following steps: the optical image is a self-luminous phenomenon, the image acquisition module carried by an aircraft acquires the optical image of the nano colloidal particles in the unknown water area state, the image processing module performs enhancement processing on the optical image by using a soluble operator based on the motion compensation principle, and the optical image distribution condition of the still water environment in an image database is compared after the optical image is displayed by the image display module to judge the turbulence degree of the water body.
CN202111494038.5A 2021-12-08 2021-12-08 Water area up-conversion fluorescence vortex detection device and detection method thereof Pending CN114076590A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114854415A (en) * 2022-03-28 2022-08-05 北京大学深圳医院 Rare earth optical probe and preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114854415A (en) * 2022-03-28 2022-08-05 北京大学深圳医院 Rare earth optical probe and preparation method and application thereof
CN114854415B (en) * 2022-03-28 2023-10-03 北京大学深圳医院 Rare earth optical probe and preparation method and application thereof

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