CN104458523B - Monitoring method for nanoscale atmospheric fine particles - Google Patents
Monitoring method for nanoscale atmospheric fine particles Download PDFInfo
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- CN104458523B CN104458523B CN201410742102.0A CN201410742102A CN104458523B CN 104458523 B CN104458523 B CN 104458523B CN 201410742102 A CN201410742102 A CN 201410742102A CN 104458523 B CN104458523 B CN 104458523B
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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
Technical field
The present invention relates to micronano optical field, particularly to a kind of monitoring side realizing nano-scale airborne fine particulate matter
Method.
Background technology
PM2.5 refers to the monitoring for a size of less than 2.5 microns fine particle concentration.Limit yet with observation method
System, at present to smaller szie：It is rarely reported especially for the monitoring method of nano-scale particle and the research of its toxicity.One side
Face, than micron particles, the particle of less nano-scale has higher bio-toxicity：Except can be through cell membrane and thin
After birth, can also pass into the more micro-cell device such as nucleus and series of chemical occurs, the synthesis of impact DNA, has more
Strong bio-toxicity is it is therefore desirable to the particle for this size carries out more intensive research.On the other hand, current
Airborne particulate detection means, excessively generally it is difficult to accomplish the Separation Research of nano-scale particle and micron particles, lacks one kind side
Just efficiently it is directed to the detection method of granule density and microphysics chemical characteristic.Because nano-scale particle sizes are less, this increasing
Accuracy and the detection accuracy of monitoring are added.
β attenuation sensors are the methods of the measurement PM2.5 of European Union's certification.β ray is attenuated, according to β after passing through particulate matter
The attenuation of ray can calculate the weight of PM2.5, according to the volume gathering sample in the identical period, draws the concentration of PM2.5.
The advantage of this method is in real time, automatically monitor can be conducive to remote observation and automatically control；Disadvantage is however that result accuracy
There is dispute, affected by factors such as composition, concentration, ambient humidities, production cost is high, and with β ray in detection process
Radiation.
Scattering spectrometry is by measuring the scattering spectrum judgement material composition of material on incident light and a kind of method of concentration,
Scattering spectrometry widely used at present is laser light scattering and white light scattering, is not applied to the prison to airborne fine particulate matter concentration
Survey.Fluorescence spectrum and Raman spectrum are laser spectrums the most commonly used, can be entered by the scattered signal intensity of material for laser light
Row quantitative analysis.In addition, high intensity laser beam can make a considerable amount of molecules in absorption species rise to excitation quantum state, therefore
Drastically increase the sensitivity of scattering spectrum, for example, use the tunable dye lasers of Nitrogen Lasers pumping to fluorescein sodium
Pulse test limit has reached 10-10Mol/L.1964, Winefordner of the U.S. etc. successfully used atomic fluorescence first
Spectroscopic assay Zn, Cd, Hg.However, the detection of the scattering spectrum with (strong) laser as light source improves testing cost and operation
Difficulty, is not therefore widely used in airborne fine particulate matter detection field.
Content of the invention
For solving above-mentioned technical problem, the present invention provides a kind of monitoring method realizing nano-scale airborne fine particulate matter,
The monitoring to nano-scale fine particle concentration, size and composition can be realized using details in a play not acted out on stage, but told through dialogues scattering spectrum technology.
The present invention solve above-mentioned technical problem adopt technical scheme be：A kind of nano-scale airborne fine particulate matter realized
Monitoring method, including：The step of the method is as follows：
Step 1, using details in a play not acted out on stage, but told through dialogues scatter image-forming principle obtain airborne fine particulate matter sample high s/n ratio have nanometer essence
The darkfield image of degree 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 particle dense
Degree；
Step 3, a certain bright spot chosen in darkfield image are fine grained, are obtained by the measurement of the details in a play not acted out on stage, but told through dialogues spectrum to this particle
Obtain its scattering spectrum data；
Step 4, by the analysis of the details in a play not acted out on stage, but told through dialogues scattering spectrum to selected target, obtain size and the composition information of this particle.
Further, using the linear dependence of details in a play not acted out on stage, but told through dialogues scattering spectrum red shift and fine particle size, and spectral information
Infer the dimension information of fine particle.
Further, also include：By changing one or more of following combination, thin to air nano-scale to realize
The monitoring of particulate matter：
(1) wavelength of incident light；
(2) spot mode of incident beam；
(3) mechanism of the scattering spectrum detecting；
(4) mode of dark-ground illumination；
(5) mode that details in a play not acted out on stage, but told through dialogues scatter imaging system scattered light is collected.
Further, also include：The size of atmospheric sounding fine particle is 100 nanometers to 2.5 microns.
The present invention provide a kind of monitoring method realizing nano-scale airborne fine particulate matter principle further illustrate as
Under：
Obtain the high letter of (by being furnished with the samplers sample of PM2.5 cutting head) aerosol sample using dark field imaging technique
Make an uproar than the darkfield image with nano-precision；Using 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, by the survey of the details in a play not acted out on stage, but told through dialogues spectrum to this particle
Amount obtains its scattering spectrum data；By the analysis of the scattering spectrum to fixing target, obtain size and the composition letter of this particle
Breath, realizes the monitoring of the physicochemical characteristics to nano-scale airborne particulate.
Preferably said method has following characteristics：
The fine grain darkfield image of air and details in a play not acted out on stage, but told through dialogues scattering spectrum are obtained using the details in a play not acted out on stage, but told through dialogues scattering system with nano-precision.
The design feature of details in a play not acted out on stage, but told through dialogues scattering system is mainly using central shadow shield or dark field condenser (conventional is parabolic condenser),
So that the central beam of light source is blocked it is impossible to from bottom to top enter object lens by sample, so that light changes approach, tilt
Be radiated on the sample of observation.Sample is met light and reflection is occurred or scatters, and the light of scattering puts in object lens, thus whole visual field
It is dark.Only the microscopical object lens of optical signals from sample scattering are collected, and enter CCD and carry out imaging acquisition high s/n ratio
Have nano-precision darkfield image or enter spectrometer system collect nano-scale fine particle scattering spectrum.
Preferably said method also includes：
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 being 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.
Preferably said method has following characteristics：
Automatic reading to bright spot in this darkfield image (nano-scale fine particle) number is realized using luminous point extraction algorithm
Take, thus obtaining the fine particle concentration of measured zone.
Preferably said method has following characteristics：
Analyze the composition information of airborne fine particulate matter using scattering spectrum.
Preferably said method has following characteristics：
Side-play amount using scattering spectrum calculates the dimension information of fine particle.The change of fine grain size can notable shadow
Ring the distribution of the details in a play not acted out on stage, but told through dialogues scattering spectrum to particle.With the increase of nanostructure size, there is red shift in the peak value of details in a play not acted out on stage, but told through dialogues scattering spectrum,
And side-play amount is linear with the change of size.The precision of the airborne fine particulate matter size of measurement nano-scale is 100 nanometers
To micron order.
Present invention advantage compared with prior art is：
This method realizing the monitoring of nano-scale airborne fine particulate matter of the present invention, has nanometer imaging precision and high noise
Than.Under identical multiple, simple microscope can see the details of 0.45um, but can see 0.2- under dark field microscope
The atomic wisp of 0.004um.With respect to the research meanses of β ray and the scattering spectrum of other optical maser wavelength, the present invention adopts
Details in a play not acted out on stage, but told through dialogues scattering technology using most common white light (mercury lamp or xenon lamp) as incident light, can reduce measurement triviality,
Save cost.The dark-field imaging adopting in the present invention and scattering light collecting device only need light source, a details in a play not acted out on stage, but told through dialogues camera lens and
Individual signal collection camera lens composition, both simple to operate, with low cost, again can be same realize that fine particle concentration automatically extracts
When, obtain size and the composition information of nanometer fine particle.Therefore have in the detection study of micro-nano size and widely grind
Study carefully prospect.
Brief description
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 are
Annular slot, 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) is to sweep
Retouch the image (SEM) of nano particle under electron microscope；Fig. 2 (b) corresponds to six sizes in Fig. 2 (a) from top to bottom and gradually increases
The details in a play not acted out on stage, but told through dialogues scattering spectrum of big nano particle, wherein l=2 and l=3 respectively to should nanostructured two kinds of backscatter modes；Fig. 2
C () is the optical imagery under dark-ground illumination for the particle of a large amount of 100-600 nano-scales.
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, wherein R be particle major axis dimension with
The ratio of minor axis dimension.
Specific embodiment
Below in conjunction with the accompanying drawings and specific embodiment further illustrates the present invention.
The present invention utilizes dark field imaging technique to obtain (by being furnished with the samplers sample of PM2.5 cutting head) aerosol sample
High s/n ratio the darkfield image with nano-precision；Using luminous point extraction algorithm, automatically read particle in darkfield image
Number, obtains measured zone granule density；Choose a certain bright spot (fine grained) in darkfield image, by the dark field light to this particle
The measurement of spectrum obtains its scattering spectrum data；By the analysis of the scattering spectrum to fixing target, obtain this particle size and
Composition information, realizes the monitoring of the physicochemical characteristics to nano-scale airborne fine particulate matter.
The specific present invention provides a kind of comprising the following steps that of monitoring method realizing nano-scale airborne fine particulate matter：
1. utilize details in a play not acted out on stage, but told through dialogues scattering image-forming principle to obtain (by being furnished with the samplers sample of PM2.5 cutting head) aerosol sample
High s/n ratio the darkfield image with nano-precision.
The present invention adopts transmission dark field to illuminate, and that is, the dark field condenser through immersion oil for the incident light incides on sample.Its knot
Structure feature is mainly using central shadow shield or dark field condenser (conventional is parabolic condenser), makes the central beam of light source
It is blocked, it is impossible to from bottom to top enter object lens by sample, so that light changes approach, being obliquely radiated at the mark of observation
In basis.Sample is met light and reflection is occurred or scatters, and the light of scattering puts in object lens, thus whole visual field is dark, such as Fig. 2
(c).Collect from the microscopical object lens of optical signals of sample scattering, enter CCD and be imaged, or enter spectrometer system and adopt
Collection.Fig. 2 (a) gives sweeping of the nanoparticle structure that under SEM, six sizes of 300nm-450nm increase successively
Retouch electron microscope (SEM) photo.The particle size that this sample is reacted with the dark-field imaging picture in Fig. 2 (c) is consistent, therefore should
Method can obtain the particle of the nanoscale image under 50 × 10 power microscopes, under the conditions of white light incidence, and this image has
Very high resolution ratio and signal to noise ratio.Fig. 1 gives the schematic diagram that details in a play not acted out on stage, but told through dialogues excites and collects, this device only by a details in a play not acted out on stage, but told through dialogues camera lens and
White light source forms, and has not only reduced acquisition cost but also easy and simple to handle.The emission spectrum that the experiment of Fig. 2 (b) nanostructured records, wherein
Six spectral lines correspond to the nanostructured that in 2 (a), six sizes increase successively respectively from top to bottom.
2. the present invention utilizes luminous point extraction algorithm, automatically reads particle number in darkfield image, obtains measured zone particle
Concentration.The darkfield image (as Fig. 2 (c)) of high s/n ratio reduces the difficulty of luminous point extraction, and this becomes the huge of dark-field imaging
Advantage.Using luminous point extraction algorithm, it is possible to achieve the automatic reading to bright spot (particle) number in this image, thus obtaining measurement
The granule density in region.The present invention to calculate the number of bright spot in image using the method for vertical+floor projection：First by image
Be converted to gray level image；Then the vertical direction in image is projected, calculate the direction comprise bright spot areal (by
Assuming the form of Gaussian Profile in the bright spot, the therefore width in these zone level directions should be at least above 2 pixels) more；Afterwards
These regions are projected in the horizontal direction, to distinguish the bright spot number in same vertical area.Project the region obtaining
Number is the number of bright spot.
3. the present invention passes through point target detection technology, obtains size and the composition of particle from the details in a play not acted out on stage, but told through dialogues scattering spectrum of particle
Feature.
The darkfield image of high accuracy and high s/n ratio is that the acquisition of target highlight spectrum brings great convenience.From sample
The light of scattering is collected by microscopical object lens, enters spectrometer system collection.Be can be seen that by the details in a play not acted out on stage, but told through dialogues scattering spectrum obtaining
Size (such as Fig. 2 (b), Fig. 3) change of grain 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 nanostructure size
Increase, there is red shift in the peak value of details in a play not acted out on stage, but told through dialogues scattering spectrum, and side-play amount is linear with the change of size.
Additionally, the different scattering spectrum distribution of different material composition correspondences.Therefore, a whole set of spectrum of point target is obtained
Composition and its chemical composition of this particle can also be judged.
We use white light as incident light, achieve details in a play not acted out on stage, but told through dialogues high-resolution imaging to the silver nanostructured of 100nm-600nm
With scattering spectrum analysis.Change the size of nanometer mechanism, the peak position of scattering spectrum there occurs line with the size increase of nanostructured
The red shift of property.
Non-elaborated part of the present invention belongs to the known technology of those skilled in the art.
Claims (4)
1. a kind of monitoring method realizing nano-scale airborne fine particulate matter is it is characterised in that include：The step of the method is such as
Under：
Step 1, scattered using details in a play not acted out on stage, but told through dialogues image-forming principle obtain airborne fine particulate matter sample high s/n ratio there is nano-precision
Darkfield image 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, a certain bright spot chosen in darkfield image are fine grained, obtain it by the measurement of the details in a play not acted out on stage, but told through dialogues spectrum to this particle
Scattering spectrum data；
Step 4, by the analysis of the details in a play not acted out on stage, but told through dialogues scattering spectrum to selected target, obtain size and the composition information of this particle.
2. as claimed in claim 1 a kind of monitoring method realizing nano-scale airborne fine particulate matter it is characterised in that utilize
Details in a play not acted out on stage, but told through dialogues scattering spectrum red shift and the linear dependence of fine particle size, are inferred the size letter of fine particle by spectral information
Breath.
3. as claimed in claim 1 or 2 a kind of monitoring method realizing nano-scale airborne fine particulate matter it is characterised in that
Also include：By changing one or more of following 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 detecting；
(4) mode of dark-ground illumination；
(5) mode that details in a play not acted out on stage, but told through dialogues scatter imaging system scattered light is collected.
4. as claimed in claim 1 or 2 a kind of monitoring method realizing nano-scale airborne fine particulate matter it is characterised in that
Also include：The size of atmospheric sounding fine particle is 100 nanometers to 2.5 microns.
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| CN105043948B (en) * | 2015-08-26 | 2017-09-22 | 清华大学 | The measuring system and measuring method of single nanoparticle particle diameter |
| CN105115864B (en) * | 2015-08-26 | 2018-01-23 | 清华大学 | The measuring method of single nanoparticle particle diameter |
| CN105115865B (en) * | 2015-08-26 | 2018-06-15 | 清华大学 | The measuring system of single nanoparticle grain size |
| CN109900700B (en) * | 2019-04-10 | 2021-11-12 | 南京邮电大学 | Method for detecting silver clusters in 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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