CN104458523A - Monitoring method for nanoscale atmospheric fine particles - Google Patents

Monitoring method for nanoscale atmospheric fine particles Download PDF

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CN104458523A
CN104458523A CN201410742102.0A CN201410742102A CN104458523A CN 104458523 A CN104458523 A CN 104458523A CN 201410742102 A CN201410742102 A CN 201410742102A CN 104458523 A CN104458523 A CN 104458523A
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particle
nano
play
told
details
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CN104458523B (en
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朱殷
陈浩
刘晓龙
杜志贵
何洋
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Academy of Opto Electronics of CAS
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Academy of Opto Electronics of CAS
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Abstract

The invention discloses a monitoring method for nanoscale atmospheric fine particles. The monitoring method comprises the following steps: obtaining a nanoscale dark field image with a high signal-noise ratio of an atmospheric fine particles sample by virtue of a dark field imaging technology; automatically reading the number of particles in the dark field image by virtue of a light-spot extraction algorithm to obtain the concentration of particles in a measurement area; selecting a certain bright spot (a fine particle) in the dark field image, measuring the dark field spectrum of the particle to form scattered spectrum data of the particle; analyzing the scattered spectrum of a fixed target to obtain the dimension and component information of the particle, thereby monitoring physical and chemical characteristics of the nanoscale atmospheric fine particles. According to the monitoring method, nano imaging precision and high signal-noise ratio are achieved, the operation is simple, the cost is low, and also the characteristics of dimension and component information and the like of the nano fine particles are obtained while automatic extraction of concentration of the atmospheric fine particles is realized.

Description

A kind of monitoring method realizing nano-scale airborne fine particulate matter
Technical field
The present invention relates to micronano optical field, particularly a kind of monitoring method realizing nano-scale airborne fine particulate matter.
Background technology
PM2.5 refers to the monitoring for being of a size of less than 2.5 microns fine particle concentration.But due to the restriction of observation method, at present to smaller szie: particularly rarely have report for the monitoring method of nano-scale particle and the research of its toxicity.On the one hand, the particle of the nano-scale less than micron particles has higher bio-toxicity: except can through cell membrane and cell membrane, the more micro-cell device series of chemical occurs such as nucleus can also be entered, affect the synthesis of DNA, there is stronger bio-toxicity, therefore need the particle for this size to carry out more intensive research.On the other hand, current airborne particulate detection means is too general, is difficult to the Separation Research of accomplishing nano-scale particle and micron particles, lacks a kind of conveniently for the detection method of granule density and microphysics chemical characteristic.Because nano-scale particle sizes is less, which increase accuracy and the detection accuracy of monitoring.
β attenuation sensors is the method for the measurement PM2.5 of European Union's certification.β ray is attenuated through after particle, just can calculate the weight of PM2.5, according to the volume of collected specimens in the identical period, draw the concentration of PM2.5 according to Beta-ray damping capacity.The advantage of this method to be monitored in real time, automatically, is conducive to remote observation and automatically controls; But shortcoming is result accuracy existence dispute, by the impact of the factors such as composition, concentration, ambient humidity, production cost is high, and with β x radiation x in testing process.
Scattering spectrometry is that the scattering spectrum by measuring material on incident light judges material composition and concentration one method, and the scattering spectrometry widely applied at present is laser light scattering and white light scattering, is not applied to the monitoring to airborne fine particulate matter concentration.Fluorescence spectrum and Raman spectrum are the laser spectrums the most generally applied, and the scattered signal intensity by material for laser light carries out quantitative test.In addition, high intensity laser beam can make a considerable amount of molecule in absorption species rise to excitation quantum state, therefore drastically increase the sensitivity of scattering spectrum, such as, reach 10 with the monopulse detectability of tunable dye lasers to uranin of Nitrogen Lasers pumping -10mol/L.1964, the Winefordner of the U.S. etc. successfully determined Zn, Cd, Hg with atomic fluorescence spectrophotometry first.But, improve testing cost and operation easier with the detection that (by force) laser is the scattering spectrum of light source, be not therefore widely used at airborne fine particulate matter detection field.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of monitoring method realizing nano-scale airborne fine particulate matter, the monitoring of details in a play not acted out on stage, but told through dialogues scattering spectrum technology realization to nano-scale fine particle concentration, size and composition can be adopted.
The technical scheme that the present invention solves the problems of the technologies described above employing is: a kind of monitoring method realizing nano-scale airborne fine particulate matter, comprising: the step of the method is as follows:
Step 1, the darkfield image with nano-precision utilizing the high s/n ratio of details in a play not acted out on stage, but told through dialogues scattering image-forming principle acquisition airborne fine particulate matter sample and details in a play not acted out on stage, but told through dialogues scattering spectrum;
Step 2, utilize luminous point extraction algorithm, automatically read particle number in darkfield image, obtain measured zone granule density;
Step 3, choose a certain bright spot in darkfield image and fine grained, obtain its scattering spectrum data by the measurement of the details in a play not acted out on stage, but told through dialogues spectrum to this particle;
Step 4, by analysis to the details in a play not acted out on stage, but told through dialogues scattering spectrum of selected target, obtain size and the composition information of this particle.
Further, details in a play not acted out on stage, but told through dialogues scattering image-forming principle is utilized to obtain the darkfield image with nano-precision and the details in a play not acted out on stage, but told through dialogues scattering spectrum of the high s/n ratio of airborne fine particulate matter sample.
Further, utilize luminous point extraction algorithm, automatically read particle number in darkfield image, obtain measured zone granule density.
Further, utilize the linear dependence of the red shift of details in a play not acted out on stage, but told through dialogues scattering spectrum and fine particle size, spectral information infers the dimension information of fine particle again.
Further, details in a play not acted out on stage, but told through dialogues scattering spectrum is utilized to infer the composition information of fine particle.
Further, also comprise: by change below in one or more combination, to realize the monitoring to air nano-scale fine particle
(1) wavelength of incident light;
(2) spot mode of incident beam;
(3) mechanism of the scattering spectrum detected;
(4) mode of dark ground illumination;
(5) mode of details in a play not acted out on stage, but told through dialogues scatter imaging system scattered light collection.
Further, also comprise: atmospheric sounding fine particle is of a size of 100 nanometers to 2.5 micron.
A kind of principle realizing the monitoring method of nano-scale airborne fine particulate matter provided by the invention further illustrates as follows:
Dark field imaging technique is utilized to obtain the darkfield image with nano-precision of the high s/n ratio of (by being furnished with the samplers sample of PM2.5 cutting head) aerosol sample; Utilize luminous point extraction algorithm, automatically read particle number in darkfield image, obtain measured zone granule density; Choose a certain bright spot (fine grained) in darkfield image, obtain its scattering spectrum data by the measurement of the details in a play not acted out on stage, but told through dialogues spectrum to this particle; By the analysis of the scattering spectrum to fixed target, obtain size and the composition information of this particle, realize the monitoring of the physicochemical characteristics to nano-scale airborne particulate.
Preferred said method has following characteristics:
The details in a play not acted out on stage, but told through dialogues scattering system with nano-precision is adopted to obtain the fine grain darkfield image of air and details in a play not acted out on stage, but told through dialogues scattering spectrum.The design feature of details in a play not acted out on stage, but told through dialogues scattering system mainly uses central shadow shield or dark field condenser (conventional is parabolic condenser), the central beam of light source is stopped, from bottom to top can not enter object lens by sample, thus make light change approach, be radiated at obliquely on the sample of observation.Sample is met light and reflection or scattering is occurred, and the light of scattering drops in object lens, and thus the whole visual field is dark.Only collect from the microscopical object lens of the optical signals of sample scattering, enter CCD and carry out the darkfield image with nano-precision of imaging acquisition high s/n ratio or enter the scattering spectrum that spectrometer system collects nano-scale fine particle.
Preferred said method also comprises:
Institute's incident light is the laser of white light and any wavelength;
Institute's incident beam is any type of spot mode;
The scattering spectrum detected is the scattering spectrum of any mechanism;
The mode of dark ground illumination is any type of incidence;
The scattered light of dark-field system is collected as any type of collection mode.
Preferred said method has following characteristics:
Adopt the automatic reading of luminous point extraction algorithm realization to bright spot in this darkfield image (nano-scale fine particle) number, thus obtain the fine particle concentration of measured zone.
Preferred said method has following characteristics:
Adopt the composition information of scattering spectrum analyse atmos fine particle.
Preferred said method has following characteristics:
The side-play amount of scattering spectrum is utilized to calculate the dimension information of fine particle.The change of fine grain size can significantly impact the distribution of the details in a play not acted out on stage, but told through dialogues scattering spectrum of particle.With the increase of nanostructure size, the peak value generation red shift of details in a play not acted out on stage, but told through dialogues scattering spectrum, and the change of side-play amount and size is linear.The precision measuring the airborne fine particulate matter size of nano-scale is that 100 nanometers are to micron order.
The present invention's advantage is compared with prior art:
This method realizing the monitoring of nano-scale airborne fine particulate matter of the present invention, has nanometer imaging precision and high s/n ratio.Under identical multiple, simple microscope can see the details of 0.45um, but can see the atomic wisp of 0.2-0.004um under dark field microscope.Relative to the research means of β ray with the scattering spectrum of other optical maser wavelength, the details in a play not acted out on stage, but told through dialogues scattering technology that the present invention adopts can adopt prevailing white light (mercury lamp or xenon lamp) as incident light, reduces the triviality of measurement, has saved cost.The dark-field imaging adopted in the present invention and scattered light gathering-device only need light source, a details in a play not acted out on stage, but told through dialogues camera lens and a signal collection camera lens composition, both simple to operate, with low cost, while automatically can extracting realizing fine particle concentration again, obtain size and the composition information of nanometer fine particle.Therefore in the detection study of micro-nano size, Research Prospects is widely had.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of transmission dark field scattering device, and wherein 1 is object lens, and 2 is sample, and 3 is dark field condenser, and 4 is annular slot, and arrow is light incident direction.
Fig. 2 is darkfield image and the details in a play not acted out on stage, but told through dialogues scattering spectrum of nano particle, and wherein scale is 200nm; Wherein Fig. 2 (a) image (SEM) that is nano particle under scanning electron microscope; Fig. 2 (b) to correspond in Fig. 2 (a) the details in a play not acted out on stage, but told through dialogues scattering spectrum of the nano particle that six sizes increase gradually from top to bottom, and wherein l=2 and l=3 is respectively to should two kinds of backscatter modes of nanostructured; The optical imagery of particle under dark ground illumination that Fig. 2 (c) is a large amount of 100-600 nano-scale.
Fig. 3 is the linear dependence of nanostructured details in a play not acted out on stage, but told through dialogues scattering spectrum and size, and wherein R is the major axis dimension of particle and the ratio of minor axis dimension.
Embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and specific embodiment.
The present invention utilizes dark field imaging technique to obtain the darkfield image with nano-precision of the high s/n ratio of (by being furnished with the samplers sample of PM2.5 cutting head) aerosol sample; Utilize luminous point extraction algorithm, automatically read particle number in darkfield image, obtain measured zone granule density; Choose a certain bright spot (fine grained) in darkfield image, obtain its scattering spectrum data by the measurement of the details in a play not acted out on stage, but told through dialogues spectrum to this particle; By the analysis of the scattering spectrum to fixed target, obtain size and the composition information of this particle, realize the monitoring of the physicochemical characteristics to nano-scale airborne fine particulate matter.
It is concrete that to the invention provides a kind of concrete steps realizing the monitoring method of nano-scale airborne fine particulate matter as follows:
1. utilize details in a play not acted out on stage, but told through dialogues scattering image-forming principle to obtain the darkfield image with nano-precision of the high s/n ratio of (by being furnished with the samplers sample of PM2.5 cutting head) aerosol sample
The present invention adopts transmission dark field to throw light on, and namely incident light incides on sample through the dark field condenser of immersion oil.Its design feature mainly uses central shadow shield or dark field condenser (conventional is parabolic condenser), the central beam of light source is stopped, from bottom to top can not enter object lens by sample, thus make light change approach, be radiated at obliquely on the sample of observation.Sample is met light and reflection or scattering is occurred, and the light of scattering drops in object lens, and thus the whole visual field is dark, as Fig. 2 (c).Collect from the microscopical object lens of the optical signals of sample scattering, enter CCD and carry out imaging, or enter spectrometer system collection.Fig. 2 (a) gives scanning electron microscope (SEM) photo of the nanoparticle structure that 300nm-450nm six sizes under scanning electron microscope increase successively.This sample is consistent with the particle size that the dark-field imaging picture in Fig. 2 (c) reacts, therefore the method can obtain the image of the particle of nanoscale under 50 × 10 power microscopes, under the incident condition of white light, and this image has very high resolution and signal to noise ratio (S/N ratio).Fig. 1 gives the schematic diagram that details in a play not acted out on stage, but told through dialogues excites and collects, not only this device is only made up of a details in a play not acted out on stage, but told through dialogues camera lens and white light source, reduces acquisition cost but also easy and simple to handle.Fig. 2 (b) nanostructured tests the emission spectrum recorded, and wherein six spectral lines distinguish the nanostructured that in corresponding 2 (a), six sizes increase successively from top to bottom.
2. the present invention utilizes luminous point extraction algorithm, automatically reads particle number in darkfield image, obtains measured zone granule density.The darkfield image (as Fig. 2 (c)) of high s/n ratio reduces the difficulty of luminous point extraction, and this becomes the huge advantage of dark-field imaging.Utilize luminous point extraction algorithm, the automatic reading to bright spot (particle) number in this image can be realized, thus obtain the granule density of measured zone.The present invention adopts the method for vertically+horizontal projection to carry out the number of bright spot in computed image: first image is converted to gray level image; Then project in the vertical direction of image, calculate the areal (because bright spot presents the form of Gaussian distribution, therefore the width in these zone level directions at least should be greater than 2 pixels) comprising bright spot in this direction more; Afterwards these regions are projected in the horizontal direction, to distinguish the bright spot number in same vertical area.The number of regions that projection obtains is the number of bright spot.
3. the present invention is by point target detection technology, obtains size and the composition characteristics of particle from the details in a play not acted out on stage, but told through dialogues scattering spectrum of particle.
The darkfield image of high precision and high s/n ratio is that the acquisition of target highlight spectrum brings great convenience.Collected by microscopical object lens from the light of sample scattering, enter spectrometer system collection.As can be seen from the details in a play not acted out on stage, but told through dialogues scattering spectrum obtained, the size of particle is (as Fig. 2 (b), Fig. 3) change can significantly impact the distribution of the details in a play not acted out on stage, but told through dialogues scattering spectrum of particle, with the increase of nanostructure size, the peak value generation red shift of details in a play not acted out on stage, but told through dialogues scattering spectrum, and the change of side-play amount and size is linear.
In addition, the scattering spectrum distribution that different material compositions is corresponding different.Therefore, composition and its chemical composition that also can judge this particle are obtained to a whole set of spectrum of point target.
We as incident light, achieve details in a play not acted out on stage, but told through dialogues high-resolution imaging and scattering spectrum analysis to the silver nanostructured of 100nm-600nm with white light.Change the size of nanometer mechanism, the peak position of scattering spectrum there occurs linear red shift with the size increase of nanostructured.
Non-elaborated part of the present invention belongs to the known technology of those skilled in the art.

Claims (7)

1. realize a monitoring method for nano-scale airborne fine particulate matter, it is characterized in that, comprising: the step of the method is as follows:
Step 1, the darkfield image with nano-precision utilizing the high s/n ratio of details in a play not acted out on stage, but told through dialogues scattering image-forming principle acquisition airborne fine particulate matter sample and details in a play not acted out on stage, but told through dialogues scattering spectrum;
Step 2, utilize luminous point extraction algorithm, automatically read particle number in darkfield image, obtain measured zone granule density;
Step 3, choose a certain bright spot in darkfield image and fine grained, obtain its scattering spectrum data by the measurement of the details in a play not acted out on stage, but told through dialogues spectrum to this particle;
Step 4, by analysis to the details in a play not acted out on stage, but told through dialogues scattering spectrum of selected target, obtain size and the composition information of this particle.
2. a kind of monitoring method realizing nano-scale airborne fine particulate matter as claimed in claim 1, is characterized in that, utilizes details in a play not acted out on stage, but told through dialogues scattering image-forming principle to obtain the darkfield image with nano-precision and the details in a play not acted out on stage, but told through dialogues scattering spectrum of the high s/n ratio of airborne fine particulate matter sample.
3. a kind of monitoring method realizing nano-scale airborne fine particulate matter as claimed in claim 1, is characterized in that, utilize luminous point extraction algorithm, automatically reads particle number in darkfield image, obtains measured zone granule density.
4. a kind of monitoring method realizing nano-scale airborne fine particulate matter as claimed in claim 1, is characterized in that, utilize the linear dependence of the red shift of details in a play not acted out on stage, but told through dialogues scattering spectrum and fine particle size, is inferred the dimension information of fine particle by spectral information.
5. a kind of monitoring method realizing nano-scale airborne fine particulate matter as claimed in claim 1, is characterized in that, utilizes details in a play not acted out on stage, but told through dialogues scattering spectrum to infer the composition information of fine particle.
6., as a kind of monitoring method realizing nano-scale airborne fine particulate matter in claim 1-5 as described in any one, it is characterized in that, also comprise: by change below in one or more combination, to realize the monitoring to air nano-scale fine particle
(1) wavelength of incident light;
(2) spot mode of incident beam;
(3) mechanism of the scattering spectrum detected;
(4) mode of dark ground illumination;
(5) mode of details in a play not acted out on stage, but told through dialogues scatter imaging system scattered light collection.
7., as a kind of monitoring method realizing nano-scale airborne fine particulate matter in claim 1-5 as described in any one, it is characterized in that, also comprise: atmospheric sounding fine particle is of a size of 100 nanometers to 2.5 micron.
CN201410742102.0A 2014-12-05 2014-12-05 Monitoring method for nanoscale atmospheric fine particles Expired - Fee Related CN104458523B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105043948A (en) * 2015-08-26 2015-11-11 清华大学 Measurement system and method for grain diameter of single nano particle
CN105115865A (en) * 2015-08-26 2015-12-02 清华大学 Measuring system for grain size of single nanometer grain
CN105115864A (en) * 2015-08-26 2015-12-02 清华大学 Single nano particle diameter measuring method
CN109900700A (en) * 2019-04-10 2019-06-18 南京邮电大学 The detection method of Silver Clusters in a kind of silicate glass
CN113567398A (en) * 2020-04-28 2021-10-29 南开大学 Lead ion concentration detection method based on dark field spectrum detection technology

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
TIMUR SHEGAI ET AL.: "Hydride Formation in Single Palladium and Magnesium Nanoparticles Studied By Nanoplasmonic Dark-Field Scattering Spectroscopy", 《ADVANCED MATERIALS》 *
成婧: "金纳米颗粒的合成及其在单粒子水平上的成像技术开发研究", 《中国博士学位论文全文数据库 工程科技I辑(月刊)》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105043948A (en) * 2015-08-26 2015-11-11 清华大学 Measurement system and method for grain diameter of single nano particle
CN105115865A (en) * 2015-08-26 2015-12-02 清华大学 Measuring system for grain size of single nanometer grain
CN105115864A (en) * 2015-08-26 2015-12-02 清华大学 Single nano particle diameter measuring method
CN105043948B (en) * 2015-08-26 2017-09-22 清华大学 The measuring system and measuring method of single nanoparticle particle diameter
CN109900700A (en) * 2019-04-10 2019-06-18 南京邮电大学 The detection method of Silver Clusters in a kind of silicate glass
CN113567398A (en) * 2020-04-28 2021-10-29 南开大学 Lead ion concentration detection method based on dark field spectrum detection technology

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