CN105043948B - The measuring system and measuring method of single nanoparticle particle diameter - Google Patents

The measuring system and measuring method of single nanoparticle particle diameter Download PDF

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CN105043948B
CN105043948B CN201510529685.3A CN201510529685A CN105043948B CN 105043948 B CN105043948 B CN 105043948B CN 201510529685 A CN201510529685 A CN 201510529685A CN 105043948 B CN105043948 B CN 105043948B
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nano particle
particle diameter
standard
particle
hot spot
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CN105043948A (en
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白本锋
肖晓飞
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Tsinghua University
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Abstract

The present invention relates to a kind of measuring system of single nanoparticle particle diameter, including a light source, objective table, object lens, convex lens, CCD and its controller, data wire and display and processing unit, the light that the light source is sent is by objective lens entrance to stage surface, and through object lens after scattering, after convex lens, it is imaged on CCD and its controller, display and processing unit are inputted through data wire, it is characterized in that, further comprise an annular diaphragm, Perimeter Truss Reflector, the light sends directional light will form hollow annular light beam after annular diaphragm, object lens will be reflected into after Perimeter Truss Reflector, effect through object lens converges to objective table.The invention further relates to the measuring method that a kind of measuring system using above-mentioned single nanoparticle particle diameter measures single nanoparticle particle diameter.

Description

The measuring system and measuring method of single nanoparticle particle diameter
Technical field
The present invention relates to field of optical measurements, nano particle is measured in particular with details in a play not acted out on stage, but told through dialogues scattering strength, is received for single Measuring system and measuring method that rice grain particle diameter is quickly measured.
Background technology
Because metal nanoparticle has the particle diameter of nanometer scale, many special effectses are made it have, such as small-size effect, Skin effect, quantum effect and macro quanta tunnel effect etc., so that its light, electricity, sound, hot and other physical characteristic tables Reveal the special nature completely different with conventional blocks material.And many characteristics of metal nanoparticle have with its particle size Substantial connection, therefore measurement to metal nanoparticle particle diameter and sign have important scientific research and Practical significance.
Main method currently used for metal nanoparticle grain diameter measurement is micro-imaging method and scatterometry method.Wherein, Micro-imaging method is to apply certain micro-imaging technique to nano particle direct imaging, and then the direct measurement on its micro-image The method of particle size.Micro-imaging method can be accurately measured the particle diameter of single metal nano particle, but needs complexity Expensive instrument and equipment, and with measuring speed is slow, the low shortcoming of efficiency;There is scatterometry method and mainly having to be divided into dynamic optical to dissipate Penetrate method, small angle x-ray scattering (SAXS) method, scattering spectrometry etc..Scatterometry method can quickly measure large sample amount nano particle Size and its distribution, but individual particle can not be measured.
In actual applications, it is desirable to achieve quickly being measured single nanoparticle, but current method is also not This demand can be met well.
The content of the invention
In summary, it is necessory to provide, a quasi-instrument and measurement cost be relatively low, simple to operate, measuring speed is fast , the measurement apparatus and method that single metal nano particle diameter can be quickly measured.
A kind of measuring system of single nanoparticle particle diameter, including a light source, objective table, object lens, convex lens, CCD and its Controller, data wire and display and processing unit, the light that the light source is sent pass through objective lens entrance to stage surface, and After scattering after object lens, convex lens, it is imaged on CCD and its controller, display and processing unit is inputted through data wire, its In, further comprise an annular diaphragm, Perimeter Truss Reflector, the light sends directional light will form hollow after annular diaphragm Annular light beam, will be reflected into object lens after Perimeter Truss Reflector, and the effect through object lens converges to objective table.
The measuring system of the single nanoparticle particle diameter further comprises that an optical filter is arranged at annular diaphragm and annular In input path between speculum.
A kind of measuring system using above-mentioned single nanoparticle particle diameter measures the measuring method of single nanoparticle particle diameter, Comprise the following steps:
Step S10, estimates the species of nano particle to be measured and the distribution of particle diameter;
Step S11, standard nano particle is dispersed on a first substrate, makes the sample of standard nano particle;
Step S12, the sample of described standard nano particle is measured using micro-imaging method, and measurement is obtained on first substrate The particle diameter of each standard nano particle of one presumptive areaSize, regard the measurement data of acquisition as benchmark;
Step S13, the first substrate for carrying standard nano particle is placed on objective table, using single nanoparticle grain The measuring system in footpath obtains the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of the presumptive area internal standard nano particle;
Step S14, handles the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of the standard nano particle obtained, obtains corresponding to each The scattering spot intensity of standard nano particle
Step S15, according to the measurement data of the particle diameter of each nano particle of acquisition and corresponding each standard nanometer The scattering spot intensity of grain, it is established that the scattering spot intensity of standard nano particleWith standard nano particle diameterBetween Corresponding relation;
Step S16, nano particle to be measured is dispersed on a second substrate, makes the sample of nano particle to be measured;
Step S17, the second substrate for carrying nano particle to be measured is placed on objective table, using single nanoparticle grain The measuring system in footpath is observed to the second substrate for carrying nano particle to be measured, obtains the scattering hot spot of nano particle to be measured Details in a play not acted out on stage, but told through dialogues micro-image;And
Step S18, according to the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of the nano particle to be measured of acquisition, obtains and corresponds to each The scattering spot intensity of nano particle to be measured, and spot intensity is scattered according to the standard for the nano particle set upWith Standard nano particle diameterBetween corresponding relation, obtain the particle diameter of nano particle to be measured in details in a play not acted out on stage, but told through dialogues micro-image
Compared with prior art, the measuring system and measuring method for the single nanoparticle particle diameter that the present invention is provided, profit With details in a play not acted out on stage, but told through dialogues scattering strength method, quick measurement can be realized to single nanoparticle measurement and light scattering method with reference to micro-imaging method Advantage, the scattering properties based on metal nanoparticle utilizes the measurement data of the sample of standard nano particle, it is established that nanometer Relation between the scattering spot intensity and nano particle diameter of particle.By measuring individual particle under details in a play not acted out on stage, but told through dialogues microscopy conditions Scatter spot intensity, you can quickly estimate its particle size, show with measurement is quick, measurement cost is cheap, operation is easy etc. Write advantage.
Brief description of the drawings
The structural representation of the measuring system 100 for the single nanoparticle particle diameter that Fig. 1 provides for first embodiment of the invention.
Fig. 2 measures feature image for the sample atom force microscope of standard nano particle.
Fig. 3 is the details in a play not acted out on stage, but told through dialogues micro-image of the sample of the standard nano particle corresponding to region shown in Fig. 2.
Fig. 4 is the binary picture that nano particle details in a play not acted out on stage, but told through dialogues scatters hot spot.
Fig. 5 is the testing result that the particle obtained through Hough transform circle detection method scatters facula position.
The structure of the measuring system 200 for the single metal nano particle diameter that Fig. 6 provides for second embodiment of the invention is shown It is intended to.
Main element symbol description
The measuring system of single nanoparticle particle diameter 100,200
Light source 1
Annular diaphragm 2
Perimeter Truss Reflector 3
Objective table 4
Object lens 5
Convex lens 6
CCD and its controller 7
Data wire 8
Display and processing unit 9
Optical filter 10
Specific examples below will further illustrate the present invention with reference to above-mentioned accompanying drawing.
Embodiment
Describe the measuring system and method for the single nanoparticle particle diameter that the present invention is provided in detail below with reference to accompanying drawing.For Convenient description, the present invention introduces the measuring system of single nanoparticle particle diameter first.
Referring to Fig. 1, first embodiment of the invention provides a kind of measuring system 100 of single nanoparticle particle diameter, it is described The measuring system 100 of single metal nano particle diameter includes a light source 1, annular diaphragm 2, Perimeter Truss Reflector 3, objective table 4, thing Mirror 5, convex lens 6, CCD and its controller 7, data wire 8, display and processing unit 9.The light 1 sends directional light by annular Hollow annular light beam will be formed after diaphragm 2, object lens 5 will be reflected into after Perimeter Truss Reflector 3, through using foreign currency for object lens 5 On the sample for gathering objective table 4.Sample can produce scattered light under the irradiation of incident light, and the scattered light of sample passes through object lens 5, convex Lens 8, are finally imaged on CCD and its controller 7.
Described light source 1 monochromatic light or approximate monochromatic light parallel to produce, are used as the illumination light of system.Light source 1 is sent out The light gone out incides the surface of objective table 4 by object lens 5, and after scattering after object lens 5, convex lens 8, in CCD and its control It is imaged on device 7 processed, display and processing unit 9 is inputted by data wire 8.Described annular diaphragm 2 is to putting down of producing light source 1 Row light shaping turns into hollow ring light beam.Hollow ring light beam is reflected into by described Perimeter Truss Reflector 3 to light path of turning back Object lens 5.In the present embodiment, the Perimeter Truss Reflector 3 is arranged between object lens 5 and convex lens 6, into entering for Perimeter Truss Reflector 3 Light is penetrated perpendicular to the emergent light from the outgoing of Perimeter Truss Reflector 3.
Described objective table 4 is used for the position for carrying sample and adjustment sample, specifically, can be with described objective table 4 Including a substrate(It is not shown)Sample to carry nano particle.Described objective table 4 can be realized to the position of sample Adjustment.The sample of nano particle is spherical metal nano particle in this example.Described substrate can be carried out according to specific experiment The quartz glass of rectangle is employed as substrate in selection, the present embodiment.
Described object lens 5 are used for collection and imaging to the scattered light of nano particle, the specific parameter of described object lens 5 It can be selected with experimental requirement and annular diaphragm 2, and the numerical aperture of Perimeter Truss Reflector 3.It is described in this example The magnifying power of object lens 5 is 100×, numerical aperture is 0.8.
Described convex lens 6 play a part of field lens, are arranged at the scattered light for the nano particle that can be collected into object lens It is imaged on CCD and its controller 7, described CCD and its controller 7 can be obtained by the details in a play not acted out on stage, but told through dialogues of the scattering hot spot of nano particle Micro-image.
Described CCD and its controller 7 are used to obtain the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of nano particle, and The darkfield image of the obtained scattering hot spot comprising nano particle is converted into electric signal, final described electric signal passes through data Line 8 reaches display and processing unit 9.
Described display and processing unit 9 are used for the electric signal for receiving the output of data wire 8, are converted into digital image data, And digital picture is handled, and then obtain the strength information of the corresponding scattering hot spot of each nano particle.Specifically, described Display and processing unit 9 is included in described CCD and its controller 7 and display and processing unit 9 obtains dissipating for nano particle The details in a play not acted out on stage, but told through dialogues micro-image of hot spot is penetrated, and digital picture is handled, and then obtains the corresponding scattering hot spot of each nano particle Strength information, database in display and processing unit 9 is so as to obtaining corresponding to each scattering in details in a play not acted out on stage, but told through dialogues micro-image The particle diameter of hot spot.
Also referring to Fig. 2-5, the invention provides a kind of measuring system 100 using the single nanoparticle particle diameter The method for measuring the particle diameter of single nanoparticle, comprises the following steps:
Step S10, estimates the species of nano particle to be measured and the distribution of particle diameter.
The species and particle diameter of the nano particle can be according to the colors of metal nanoparticle, or according to metal nano The electron microscopic picture of grain is estimated, and can determine whether the species of metal nanoparticle and the substantially distribution of particle diameter.The metal is received The species of rice grain is the general face shaping of the metal nanoparticle.In the present embodiment, the metal nanoparticle Species be spherical or subsphaeroidal gold nano grain.
Step S11, standard nano particle is dispersed on substrate, makes the sample of standard nano particle.
Because nano particle is collosol state, and it need to be deposited on substrate and dry applied to the nano particle of this method, And to scatter well, it is to avoid reunite.Therefore, the present embodiment is entered using following operating process to the sample of standard nano particle Row prepares:
1)Cleaning removes the organic matter of substrate surface;
2)Cleaning removes the inorganic matter of substrate surface;
3)Hydrophilic treated is carried out to substrate surface, the hydrophilic active of substrate surface is improved, now the surface state of substrate is very It is adapted to the deposition of other chemical materials;
4)In order to more stably grab attached nano particle, one layer of APTES of self assembly on aforesaid substrate surface, i.e., in APTES In solution soak 30 minutes, after eluted with isopropanol;
5)Above-mentioned treated substrate is immersed in the aqueous solution of gold nano grain, about 4 hours.Substrate is taken out, is used Water wash.
So far, nano particle scatter on substrate, in subsequent step, and we are by the standard nanometer on this substrate Grain is measured.
For the particle diameter of more accurate measurement nano particle to be measured, herein for making the sample of standard nano particle Standard nano particle particle size range will as far as possible close to nano particle to be measured particle size range.Described standard nano particle Can be sampling observation nano particle to be measured or the different batches made using same process, the nano particle of different manufacturers 's.In this example, use and inspect nano particle to be measured by random samples.
Step S12, the sample of described standard nano particle is measured using micro-imaging method, and measurement obtains making a reservation on substrate The particle diameter of each standard nano particle in regionSize, regard measurement data as benchmark.
Single standard nano particle is imaged using micro-imaging method, so that the micro-image of standard nano particle is obtained, The particle diameter of single standard nano particle can be obtained by by the processing of the micro-image to standard nano particle.This example In, we employ AFM and measure described standard nano particle, obtain each mark of presumptive area on substrate The particle diameter of quasi- nano particle, and this measurement data is used in follow-up system calibrating.
The principle that described region is chosen is:
1. choose region it is as larger as possible, comprising nano particle particle size range it is as big as possible;
2. selected by region to have easy positioning, be this in the manufacturing process of foregoing print, can be on substrate Marked accordingly.
Step S13, the standard nano particle in region is obtained using the measuring system 100 of single metal nano particle diameter Scattering hot spot details in a play not acted out on stage, but told through dialogues micro-image.
The details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of the standard nano particle can be obtained by following steps:
Step S131, the described substrate of standard nano particle that is loaded with is placed on objective table 6, opens lighting source, The relative position of annular diaphragm, Perimeter Truss Reflector and object lens 7 and objective table is adjusted, is obtained by display and the observation of processing unit 11 The image taken, until obtaining observing the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of standard nano particle;
Step S132, then, adjusts objective table 6, and observes the image obtained by display and processing unit 11, until seeking Find the region of step S12 measurements;And
Step S133, is obtained by described image processing software and preserves the scattering of the standard nano particle in presumptive area The details in a play not acted out on stage, but told through dialogues micro-image of hot spot.
The details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot for the standard nano particle that step S14, process step S13 are obtained, acquisition pair Should be in the scattering spot intensity of each standard nano particle
In actual measurement, the absolute intensity for wanting accurately to measure nano particle scattered light is highly difficult.But according to diffraction Theory is understood, scatters spot intensityIt can be used to reflect the size of particle scattered light intensity.Software can be handled by described image The details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of the step S13 standard nano particles obtained is handled:
1)Image is pre-processed, the noise reduction process to image is realized;
2)Original color image is processed as gray-scale map;
3)Gray-scale map is converted into binary map using Binarization methods;
4)Detection to single scattering facula position;
5)The gray scale of all pixels point of each scattering hot spot being detected is extracted, and summed, is obtained The scattering spot intensity of each particle.
In this example, realized using Niblack Binarization methods and gray-scale map is converted into binary map, using Hough transform Circle detection method realizes the detection to single scattering facula position.
Step S15, is obtained according to the measurement data of the particle diameter of the step S12 each nano particles obtained with step S14 The scattering spot intensity of corresponding each standard nano particle, it is established that the scattering spot intensity of standard nano particleWith mark Quasi- nano particle diameterBetween corresponding relation.
According to the relative position of standard nano particle, by the particle diameter of the step S12 each standard nano particles obtained's The scattering spot intensity of measurement data and the step S14 corresponding each standard nano particles obtainedCorresponded to, used The mode of data fitting sets up the scattering spot intensity of the standard nano particle under this experiment conditionWith nano particle grain FootpathBetween relation.
Influence in view of different approximating methods to measurement result, the level selection principle of polynomial fitting is as follows:
1)If in calibration process, the particle size range of standard particle covers the particle size range of testing sample, then using high Level fitting of a polynomial more meets experimental data, and the measurement accuracy to candidate particles is also higher;
2)If in calibration process, the particle size range of standard particle is not covered by the particle size range of testing sample, when using senior When order polynomial is fitted, due to the fluctuation of high-order moment, particle diameter can be caused not to be measured in standard sample particle size range There is certain deviation in the measurement of particle, i.e., this situation is beyond calibration range.In the case, a fitting of a polynomial result To more it stablize, reliably.
Summary considers to determine that optimal fitting scheme realizes that step is as follows:
Step 1:, it is necessary to extract the particle diameter maximum and minimum value of standard particle and its corresponding in calibration process Scatter the intensity of hot spot;
Step 2:The scattering hot spot strength information of nano particle to be measured is extracted, and nano particle is sorted out:In above-mentioned scattering Particle in the strength range of hot spot and not particle within the range;
Step 3:High order is respectively adopted and a fitting of a polynomial relation calculates the particle diameter of above-mentioned two groups of particles, obtains final Measurement result.
Obviously, high-order moment fit correlation can ensure the particle diameter of the particle in the strength range of above-mentioned scattering hot spot Measurement result is more accurate, and a fitting of a polynomial relation can be prevented caused by the fluctuation of high-order moment not in the model The measurement result deviation of particle in enclosing is bigger than normal.
Step S16, nano particle to be measured is dispersed on substrate, makes the sample of nano particle to be measured.
Using the operating process in step S11, nano particle to be measured is dispersed on substrate, nano particle to be measured is made Sample.
Step S17, the scattered light of nano particle to be measured is obtained using the measuring system 100 of single metal nano particle diameter The details in a play not acted out on stage, but told through dialogues micro-image of spot.
The substrate of standard nano particle that is loaded with described in step S13 is replaced by after the substrate of nano particle to be measured, adjusted The relative position of whole dark field condenser module 20 and object lens 7 and objective table, observes what is obtained by display and processing unit 11 Image, until obtaining observing the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of nano particle.Obtained by software and preserve to be measured receive The details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of rice grain.The area of the nano particle of measurement is big as far as possible according to requirement of experiment, with Obtain the scattering hot spot of the nano particle to be measured of large sample amount.
Step S18, according to the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of the step S17 nano particles to be measured obtained, acquisition pair Should be in the scattering spot intensity of each nano particle to be measured, and dissipating according to the step S15 standard nano particles set up Penetrate spot intensityWith nano particle diameterBetween relation, obtain the particle diameter of nano particle to be measured in details in a play not acted out on stage, but told through dialogues micro-image
Similar to step S14, dissipating for the nano particle to be measured that software is obtained to process step S17 is handled by described image The details in a play not acted out on stage, but told through dialogues micro-image of hot spot is penetrated, the scattering spot intensity for corresponding to each nano particle to be measured is obtained.It will obtain herein Data substitute into the scattering spot intensity of nano particle that step S15 is set upWith nano particle diameterBetween correspondence Relation, finally gives the particle diameter of single nano particle to be measured.This data is preserved for follow-up display, processing etc..
Step S11 makes the sample of standard nano particle, and the standard nano particle that is measured in step S12 particle diameter Data are only operated once, the sample of standard nano particle and the data measured can be preserved into reuse afterwards, and no longer The master sample of described nano particle is measured using micro-imaging method, the efficiency subsequently measured, the measurement of reduction is greatly improved Cost.
Also referring to Fig. 6, second embodiment of the invention provides a kind of measurement system of single metal nano particle diameter 200, the measurement of the single metal nano particle diameter is 200 to include a light source 1, and annular diaphragm 2, optical filter 10, annular is anti- Mirror 3, objective table 4, object lens 5, convex lens 6, CCD and its controller 7 are penetrated, data wire 8 is shown and processing unit 9.The single gold The measurement of metal nano-particle particle diameter be 200 structure and first embodiment described in single metal nano particle diameter measurement system 100 structure is essentially identical, and its difference is, optical filter 10 is added in light path.In the present embodiment, the optical filter 10 is set It is placed in the input path between annular diaphragm 2 and the Perimeter Truss Reflector 3.It is appreciated that described optical filter 10 can be with It is placed on the other positions of input path.
The details in a play not acted out on stage, but told through dialogues scattering strength method quickly measured provided by the present invention for single nanoparticle particle diameter, with reference to micro-imaging Method can realize the advantage quickly measured to single nanoparticle measurement and light scattering method.Scattering based on metal nanoparticle Characteristic, utilizes the measurement data of the sample of standard metal nano particle, it is established that the scattering spot intensity and nanometer of nano particle Relation between grain diameter.By measuring scattering spot intensity of the individual particle under details in a play not acted out on stage, but told through dialogues microscopy conditions, you can quickly estimate Count out its particle size.Devising corresponding software realizes to the aobvious of the details in a play not acted out on stage, but told through dialogues micro-image for scattering hot spot of nano particle Show, obtain, automatically processing, preserving and data follow-up processing.Step S11 and step S12 of the present invention need to only be operated once, Without being measured using micro-imaging method to the sample of standard nano particle in subsequent experimental.Therefore, this method has Measure the ability of single metal nano particle diameter, and with that measurement is quick, measurement cost is cheap, operation is easy etc. is notable excellent Point.
In addition, those skilled in the art can also make other changes in spirit of the invention, these are according to present invention essence certainly The change that god is made, should all be included in scope of the present invention.

Claims (10)

1. a kind of measuring system of single nanoparticle particle diameter, including a light source, objective table, object lens, convex lens, CCD and its control Device processed, data wire and display and processing unit, the light that the light source is sent pass through objective lens entrance to stage surface, and pass through Cross after scattering after object lens, convex lens, be imaged on CCD and its controller, display and processing unit are inputted through data wire, it is special Levy and be, further comprise an annular diaphragm, and a Perimeter Truss Reflector, the light sends directional light after annular diaphragm by shape Into hollow annular light beam, object lens are reflected into after Perimeter Truss Reflector, the effect through object lens converges to objective table.
2. the measuring system of single nanoparticle particle diameter as claimed in claim 1, it is characterised in that further comprise an optical filtering Piece is arranged in the input path between annular diaphragm and Perimeter Truss Reflector.
Received 3. a kind of measuring system measurement of the single nanoparticle particle diameter in utilization claim 1-2 described in any one is single The measuring method of rice grain particle diameter, comprises the following steps:
Step S10, estimates the species of nano particle to be measured and the distribution of particle diameter;
Step S11, standard nano particle is dispersed on a first substrate, makes the sample of standard nano particle;
Step S12, measures the sample of described standard nano particle using micro-imaging method, and it is pre- that measurement obtains on first substrate one Determine the particle diameter D sizes of each standard nano particle in region, regard the measurement data of acquisition as benchmark;
Step S13, the first substrate for carrying standard nano particle is placed on objective table, using single nanoparticle particle diameter Measuring system obtains the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of the presumptive area internal standard nano particle;
Step S14, handles the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of the standard nano particle obtained, obtains and correspond to each standard The scattering hot spot intensity I nt of nano particleλ
Step S15, according to the measurement data of the particle diameter of each nano particle of acquisition and corresponding each standard nano particle Scatter spot intensity, it is established that the scattering hot spot intensity I nt of standard nano particleλWith pair between standard nano particle diameter D It should be related to;
Step S16, nano particle to be measured is dispersed on a second substrate, makes the sample of nano particle to be measured;
Step S17, the second substrate for carrying nano particle to be measured is placed on objective table, using single nanoparticle particle diameter Measuring system is observed to the second substrate for carrying nano particle to be measured, and obtain nano particle to be measured scatters the dark of hot spot Field micro-image;And
Step S18, according to the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of the nano particle to be measured of acquisition, is obtained corresponding to each to be measured The scattering hot spot intensity I nt ' of nano particleλ, and hot spot intensity I nt is scattered according to the standard for the nano particle set upλWith standard Corresponding relation between nano particle diameter D, obtains the particle diameter D ' of nano particle to be measured in details in a play not acted out on stage, but told through dialogues micro-image.
4. the measuring method of single nanoparticle particle diameter as claimed in claim 3, it is characterised in that the standard nano particle First substrate is dispersed in the following manner:
Cleaning removes the organic matter on first substrate surface;
Cleaning removes the inorganic matter on first substrate surface;
Doing hydrophilic treated to first substrate surface makes first substrate surface have hydrophilic active, to be adapted to the heavy of standard nano particle Product;
One layer of APTES of self assembly on above-mentioned water-wetted surface, more stably to grab attached nano particle;And
Above-mentioned treated substrate is immersed in the aqueous solution of standard nano particle, after certain time, first substrate is taken out, uses Water wash.
5. the measuring method of single nanoparticle particle diameter as claimed in claim 3, it is characterised in that use AFM The sample of the described standard nano particle of measurement, obtains the particle diameter D of each standard nano particle of presumptive area on first substrate, And this measurement data is used in follow-up system calibrating.
6. the measuring method of single nanoparticle particle diameter as claimed in claim 3, it is characterised in that the standard nano particle The details in a play not acted out on stage, but told through dialogues micro-image of scattering hot spot included:
The described first substrate for being loaded with standard nano particle is placed on objective table, lighting source is opened, ring light is adjusted The relative position of door screen, Perimeter Truss Reflector and object lens and objective table, the image obtained is observed by display and processing unit, until Obtain the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of standard nano particle;
Objective table is adjusted, and the image obtained is observed by display and processing unit, until searching out described presumptive area:With And
The details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot corresponding to presumptive area is obtained and preserved by an image processing software.
7. the measuring method of single nanoparticle particle diameter as claimed in claim 6, it is characterised in that handled by described image The details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot for the standard nano particle that software processing is obtained includes:
Image is pre-processed, the noise reduction process to image is realized;
Original color image is processed as gray-scale map;
Gray-scale map is converted into binary map using Binarization methods;
Detection to single scattering facula position;And
The gray scale of all pixels point of each scattering hot spot being detected is extracted, and summed, each mark is obtained The scattering spot intensity of quasi- nano particle.
8. the measuring method of single nanoparticle particle diameter as claimed in claim 3, it is characterised in that the side being fitted using data Formula sets up the scattering hot spot intensity I nt of standard nano particleλWith the relation between standard nano particle diameter D, the data It is to the level selection principle of polynomial fitting in fit procedure:
If in calibration process, the particle size range of standard particle covers the particle size range of testing sample, then multinomial using high level Formula fitting more meets experimental data;
If in calibration process, the particle size range of standard particle is not covered by the particle size range of testing sample, when multinomial using high level When formula is fitted, due to the fluctuation of high-order moment so that the survey of the candidate particles of particle diameter not in standard sample particle size range There is certain deviation in amount, i.e., this situation is beyond calibration range, then using a fitting of a polynomial.
9. the measuring method of single nanoparticle particle diameter as claimed in claim 8, it is characterised in that intend in data fit procedure Conjunction scheme comprises the following steps:
In calibration process, the particle diameter maximum and minimum value and its corresponding scattering hot spot of standard nano particle are extracted Intensity;
The scattering hot spot strength information of nano particle to be measured is extracted, and nano particle to be measured is sorted out:In above-mentioned scattering hot spot Particle in strength range and not particle within the range;
High order is respectively adopted and a fitting of a polynomial relation calculates the particle diameter of above-mentioned two classes particle, final measurement knot is obtained Really.
10. the measuring method of single nanoparticle particle diameter as claimed in claim 3, it is characterised in that the nanometer to be measured The particle diameter D ' of grain is obtained in the following manner:
The details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of the nano particle to be measured obtained is handled by an image processing software, is corresponded to In the scattering hot spot intensity I nt ' of each nano particle to be measuredλ, the data obtained herein are substituted into the standard nanometer set up The scattering hot spot intensity I nt of grainλWith the corresponding relation between standard nano particle diameter D, single nanometer to be measured is finally given The particle diameter D ' of grain.
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