CN105115865B - The measuring system of single nanoparticle grain size - Google Patents
The measuring system of single nanoparticle grain size Download PDFInfo
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- CN105115865B CN105115865B CN201510529595.4A CN201510529595A CN105115865B CN 105115865 B CN105115865 B CN 105115865B CN 201510529595 A CN201510529595 A CN 201510529595A CN 105115865 B CN105115865 B CN 105115865B
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Abstract
The present invention relates to a kind of measuring systems of single nanoparticle grain size, including a light source, one dark field condenser module, one objective table, one object lens, one convex lens, one CCD and its controller, a data line and a display and processing unit are arranged at intervals successively, wherein, the monochromatic light that the light source is sent out becomes hollow light cone after dark field condenser module shaping, it is irradiated on objective table and generates scattering light, scattering light is by object lens, convex lens, it is finally imaged on CCD and its controller, and passes through data line transfer to display and processing unit.
Description
Technical field
The present invention relates to field of optical measurements, measure nano particle in particular with details in a play not acted out on stage, but told through dialogues scattering strength, are received for single
The measuring system and measuring method that rice grain grain size quickly measures.
Background technology
Due to metal nanoparticle have nanometer scale grain size, make it have many special effects, as small-size effect,
Skin effect, quantum effect and macro quanta tunnel effect etc., so as to make its light, electricity, sound, heat 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 grain size and characterization 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 directly measured on its micro-image
The method of particle size.Micro-imaging method can accurately measure, but need complexity the grain size of single metal nano particle
Expensive instrument and equipment, and there is measuring speed is slow, efficiency is low etc.；There is scatterometry method again mainly to have to be divided into dynamic optical and 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 practical applications, it is desirable to achieve single nanoparticle is quickly measured, but current method is also not
This demand can be met well.
Invention content
In conclusion it is necessory to provide, a kind of instrumentation and testing advantage of lower cost, easy to operate, measuring speed is fast
, can be to measuring device and method that single metal nano particle diameter quickly measures.
A kind of measuring system of single nanoparticle grain size, including a light source, a dark field condenser module, an objective table,
One object lens, a convex lens, a CCD and its controller, a data line and a display and processing unit are arranged at intervals successively,
In, the monochromatic light that the light source is sent out becomes hollow light cone after dark field condenser module shaping, is irradiated on objective table simultaneously
Generate scattering light, by object lens, convex lens is finally imaged scattering light on CCD and its controller, and pass through data line transfer to
Display and processing unit.
Compared with prior art, the measuring system of single nanoparticle grain size provided by the invention, is scattered using details in a play not acted out on stage, but told through dialogues
Intensity method, with reference to micro-imaging method can to single nanoparticle measure and light scattering method can realize quick measurement the advantages of, base
In the scattering properties of metal nanoparticle, the measurement data of the sample of standard nano particle is utilized, it is established that nano particle dissipates
Penetrate the relationship between spot intensity and nano particle diameter.By measuring scattering hot spot of the individual particle under details in a play not acted out on stage, but told through dialogues microscopy conditions
Intensity, you can quickly estimate its particle size, have and measure the remarkable advantages such as quick, measurement cost is cheap, operation is easy.
Description of the drawings
Fig. 1 is the structure diagram of the measuring system of single nanoparticle grain size that first embodiment of the invention provides.
The sample atom force microscope of Fig. 2 standard nano particles measures feature image.
Fig. 3 corresponds to the details in a play not acted out on stage, but told through dialogues micro-image of the sample of the standard nano particle in 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 of particle scattering facula position obtained through Hough transform circle detection method.
Fig. 6 is the relationship between the scattering spot intensity of nano particle and nano particle diameter.
Fig. 7 is the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of nano particle to be measured.
Fig. 8 is the distribution histogram and partial enlarged view of nano particle diameter to be measured.
Fig. 9 is the structure diagram of the measuring system of single nanoparticle grain size that second embodiment of the invention provides.
Main element symbol description
| The measuring system of single nanoparticle grain size | 100,200 |
| Dark field condenser module | 20 |
| Light source | 1 |
| Diaphragm | 2 |
| Concentrator | 3 |
| Objective table | 4 |
| Object lens | 5 |
| Convex lens | 6 |
| CCD and its controller | 7 |
| Data line | 8 |
| Display and processing unit | 9 |
| Dark field condenser | 10 |
Specific examples below will be further illustrated the present invention with reference to above-mentioned attached drawing.
Specific embodiment
Below with reference to the measuring system and method for the attached drawing single nanoparticle grain size that the present invention will be described in detail provides.For
Facilitate description, the present invention introduces the measuring system of single nanoparticle grain size first.
Referring to Fig. 1, first embodiment of the invention provides a kind of measuring system 100 of single nanoparticle grain size, it is described
The measuring system 100 of single nanoparticle grain size includes a light source 1, and a dark field condenser module 20, objective table 4, object lens 5 are convex
Lens 6, CCD and its controller 7, data line 8 and display and processing unit 9.The dark field condenser module 20, objective table 4,
The light path that object lens 5, convex lens 6, CCD and its controller 7 are exported along the light source 1 is arranged at intervals successively.What the light source 1 was sent out
Light becomes hollow light cone after 20 shaping of dark field condenser module, is irradiated on the sample on objective table 4, sample can be in incidence
Generate scattering light under the irradiation of light, the scattering light of sample is by object lens 5, convex lens 6, finally on CCD and its controller 7 into
Picture, and pass through data line 8 and be transferred to display and processing unit 9.
The light source 1 is generating monochromatic light or approximate monochromatic light, the illumination light as system.It is described in this example
Light source 1 include a photodiode, to generate approximate monochromatic light source.The light source 1 can also be other monochromatic sources or
Approximate monochromatic light source.
The dark field condenser module 20 is set to from the monochromatic light path that light source 1 is emitted, to light source 1 is defeated
The monochromatic light and approximate monochromatic light shaping gone out becomes hollow light cone, to realize dark-ground illumination.In the present embodiment, the details in a play not acted out on stage, but told through dialogues gathers
Light device module 20 includes a diaphragm 2 and concentrator 3 is set gradually.The numerical aperture complex of the dark field condenser module 20
The parameter of mirror 5 is selected, to realize dark-ground illumination.In this example, the diaphragm 2 of composition dark field condenser module 20 is
The round copper sheet of a diameter of 21mm, the numerical aperture of the concentrator 3 is 0.9.
The objective table 4 is set to from the light path for the light that dark field condenser module 20 is emitted, for carry sample and
The position of sample is adjusted, specifically, a substrate can be included on the objective table 4（It is not shown）To carry nano particle
Sample.The objective table 4 can realize the adjustment to the position of sample.In this example, the sample of the nano particle is ball
Shape metal nanoparticle.The substrate can be selected according to specific experiment, and the quartz of rectangle is employed in the present embodiment
Glass is as substrate.
The object lens 5 are set to from the light path for the light that objective table 4 is emitted, for the receipts of the scattering light to nano particle
Collection and imaging, the specific parameter of the object lens 5 can experimental requirement and the numerical aperture of dark field condenser module 20
It is selected.In this example, the magnifying power of the object lens 5 is 100 times, numerical aperture 0.8.
The convex lens 6 is set to from the light path that object lens 5 are emitted, and plays the role of field lens, and object lens 5 are collected
To the scattering light of nano particle be imaged on CCD and its controller 7, the CCD and its controller 7 can be obtained by nanometer
The details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of particle.
The 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 obtained darkfield image of the scattering hot spot comprising nano particle is converted into electric signal, the final electric signal passes through data
Line 8 reaches display and processing unit 9.
The display and processing unit 9 are used to receive the electric signal of the output of data line 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.It is specifically, described
Display and processing unit 9 is included in the 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, the database in display and processing unit 9 is so as to obtain corresponding to each scattering in details in a play not acted out on stage, but told through dialogues micro-image
The grain size of hot spot.
Also referring to Fig. 2-8, the present invention provides a kind of measuring systems 100 using the single nanoparticle grain size
The method for measuring the grain size of single nanoparticle, includes the following steps：
Step S10 estimates the type of nano particle to be measured and the distribution of grain size.
In the present embodiment, the nano particle to be measured is metal nanoparticle, therefore the type of the nano particle to be measured
And grain size can the color according to metal nanoparticle or the electron microscopic picture according to metal nanoparticle estimated, can sentence
The type of disconnected metal nanoparticle and the substantially distribution of grain size.The type of the metal nanoparticle is that the metal is received
The general face shaping of rice grain.In the present embodiment, the type of the metal nanoparticle is spherical or subsphaeroidal gold nano
Particle.
Standard nano particle is dispersed on a first substrate by step S11, makes the sample of standard nano particle.
In the present embodiment, since nanoparticle sample is collosol state, and nano particle need to precipitate on the first substrate simultaneously
It is dry, and to scatter well, it avoids reuniting.Therefore, the present embodiment uses following operating process to standard nano particle
Sample is prepared：
1）Cleaning removes the organic matter on first substrate surface；
2）Cleaning removes the inorganic matter on first substrate surface；
3）The table that hydrophilic treated makes first substrate surface have hydrophilic active, at this time first substrate is made to first substrate surface
Face state is very suitable for the deposition of other chemical materials；
4）One layer of APTES of self assembly on above-mentioned water-wetted surface, more stably to grab attached nano particle, you can in APTES
In solution by first substrate impregnate 30 minutes, after eluted with isopropanol；
5）Above-mentioned processed first substrate is immersed in the aqueous solution of gold nano grain, certain time such as about 4 is small
Shi Hou takes out first substrate, uses water wash.
So far, standard nano particle scatter on the first substrate, will be to the mark on this first substrate in subsequent step
Quasi- nanoparticle sample measures.
For the grain size of more accurate measurement nano particle to be measured, it is used to make the sample of standard nano particle herein
The particle size range of standard nano particle will be as possible close to the particle size range of nano particle to be measured.The standard nano particle
The different batches that can be sampling observation nano particle to be measured or same process is used to make, the nano particle of different manufacturers
's.In this example, using sampling observation nano particle to be measured.
Step S12, the sample of the standard nano particle is measured using micro-imaging method, and measurement is obtained on first substrate
The grain size of each standard nano particle of one presumptive areaSize, using measurement data as benchmark.
Single nanoparticle is imaged using micro-imaging method, so as to obtain the micro-image of standard nano particle, is passed through
It can be obtained by the grain size of single nanoparticle to the processing of the micro-image of standard nano particle.In this example, using original
Sub- force microscope measures the sample of the standard nano particle, obtains each standard nanometer of presumptive area on first substrate
The grain size of particle, and by this measurement data in subsequent system calibrating.
The principle that the presumptive area 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. region selected by easily positions, can be on the first substrate thus in the manufacturing process of aforementioned print
It is marked accordingly.
The first substrate for carrying standard nano particle is placed on objective table by step S13, using single nanoparticle grain
The measuring system 100 of diameter obtains the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of the specific region internal standard nano particle.
The first substrate for being loaded with standard nano particle is placed on objective table 4, opens lighting source, adjustment is dark
The relative position of field concentrator module 20 and object lens 5 and objective table 4, the image obtained by display and the observation of processing unit 9,
Until obtain 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.Then, objective table 4 is adjusted, and is passed through aobvious
Show and processing unit 9 observes the image obtained, until searching out the specific region.Software is handled by described image to obtain
And preserve the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot corresponding to specific region.
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 in step S14, processing step S13, obtains
Corresponding to the scattering spot intensity of each standard nano particle。
In practical measurement, the absolute intensity that accurately measure nano particle scattering light is highly difficult.But it is managed according to diffraction
By it is found that the scattering spot intensity of standard particleIt can be used to the size for reflecting particle scattered light intensity.At described image
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 that reason software processing steps S13 is obtained includes：
1）Image is pre-processed, realizes the noise reduction process to image；
2）It is gray-scale map by original color image processing；
3）Gray-scale map is converted into binary map using Binarization methods；
4）Detection to single scattering facula position；
5）Each gray scale of all pixels point of scattering hot spot being detected is extracted, and sum, is obtained
The scattering spot intensity of each standard nano 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 grain size of the step S12 each standard nano particles obtained with step S14
The scattering spot intensity of the corresponding each standard nano particle obtained, it is established that the scattering spot intensity of standard nano particle
With standard nano particle diameterBetween relationship.
According to the relative position of standard nano particle, the grain size of each standard nano particle that step S12 is obtained's
The scattering spot intensity of corresponding each standard nano particle that measurement data is obtained with step S14It is corresponded to, is used
The mode of data fitting sets up the scattering spot intensity of standard nano particle under this experiment conditionWith standard nanometer
Grain grain sizeBetween relationship.In view of influence of the different approximating methods to measurement result, here to the level of polynomial fitting
Selection principle is：
1）If in calibration process, the particle size range of standard particle covers the particle size range of sample to be tested, then using high
Level fitting of a polynomial more meets experimental data, to the measurement accuracy of candidate particles also higher；
2）If in calibration process, the particle size range of standard particle is not covered by the particle size range of sample to be tested, when using advanced
When order polynomial is fitted, due to the fluctuation of high-order moment, it can so that grain size is not to be measured in standard sample particle size range
There is certain deviation in the measurement of particle, i.e. this situation has exceeded calibration range, using a fitting of a polynomial.In the case,
Fitting of a polynomial result will more be stablized, is reliable.
Summary considers, determines that the realization step of optimal fitting scheme is as follows：
Step 1：In calibration process, need to extract the grain size maximum value of standard particle and minimum value and its corresponding
Scatter the intensity of hot spot；
Step 2：The scattering spot intensity information of nano particle to be measured is extracted, and nano particle to be measured is sorted out：Above-mentioned
Scatter the particle and not particle in the range in the strength range of hot spot；
Step 3：High order is respectively adopted and a fitting of a polynomial relationship calculates the grain size of above-mentioned two groups of particles, obtains final
Measurement result.
Obviously, high-order moment fit correlation can ensure the grain size of the particle in the strength range of above-mentioned scattering hot spot
Measurement result is more accurate, and a fitting of a polynomial relationship 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.
Nano particle to be measured is dispersed on a second substrate by step S16, makes the sample of nano particle to be measured.
The operating process in step S11 can be used, nano particle to be measured is dispersed on second substrate, make nanometer to be measured
The sample of particle.
The second substrate for carrying nano particle to be measured is placed on objective table 4, using single nanoparticle by step S17
The measuring system 100 of grain size is observed the second substrate for carrying nano particle to be measured, obtains dissipating for nano particle to be measured
Penetrate the details in a play not acted out on stage, but told through dialogues micro-image of hot spot.
The first substrate for being loaded with standard nano particle described in step S13 is changed to and carries nano particle to be measured
The relative position of second substrate, adjustment dark field condenser module 20 and object lens 5 and objective table 4, passes through display and processing unit 9
The image obtained is observed, 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 to be measured.It is obtained by software
Take and preserve the details in a play not acted out on stage, but told through dialogues micro-image of the scattering hot spot of nano particle to be measured.The area of the nano particle of measurement is according to requirement of experiment
It is big as far as possible, to 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
It should be in the scattering spot intensity of each nano particle to be measured, and according to the step S15 standard nano particles set up
Scatter spot intensityWith standard nano particle diameterBetween relationship, obtain nanometer to be measured in details in a play not acted out on stage, but told through dialogues micro-image
The grain size of grain。
Similar to step S14, software dissipating to the processing step S17 nano particles to be measured obtained 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, obtains the scattering spot intensity for corresponding to each nano particle to be measured.It will obtain herein
Data substitute into the scattering spot intensities of standard nano particle set up of step S15With standard nano particle diameter
Between relationship, finally obtain the grain size of single nano particle to be measured.This data is preserved for subsequent display, place
Reason etc..
Step S11 makes the grain size of standard nano particle that is measured in the sample of standard nano particle and step S12
Data only operate once, can the sample of standard nano particle and the data measured be preserved reuse later, and no longer
The master sample of the nano particle is measured using micro-imaging method, greatly improves the efficiency subsequently measured, the measurement of reduction
Cost.
Provided by the present invention for the details in a play not acted out on stage, but told through dialogues scattering strength method that single nanoparticle grain size quickly measures, with reference to micro-imaging
The advantages of method can measure single nanoparticle and light scattering method can realize quick measurement.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
Relationship 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 the subsequent processing of data.Step S11 and step S12 of the present invention need to only be operated once,
Without micro-imaging method is being used to measure the sample of standard nano particle in subsequent experimental.Therefore, this method has
Measure the ability of single metal nano particle diameter, and notable excellent with measuring that quick, measurement cost is cheap, operation is easy etc.
Point.
Also referring to Fig. 9, second embodiment of the invention provides a kind of measuring system 200 of single nanoparticle grain size,
The measuring system 200 of the single nanoparticle grain size includes a light source 1, a dark field condenser module 20, concentrator 3, loading
Platform 4, object lens 5, convex lens 6, CCD and its controller 7, data line 8 and display and processing unit 9.The single nanoparticle
The structure base of the measuring system 100 of single nanoparticle grain size described in the structure and first embodiment of the measuring system 200 of grain size
This is identical, and difference is, the dark field condenser module 20 is a dark field condenser, and the dark field condenser can be to throw
Object plane condenser, cardioid condenser, concentric spherical condenser etc..
In addition, those skilled in the art can also make other variations in spirit of the invention, these are smart according to the present invention certainly
The variation that god is made should be all included in scope of the present invention.
Claims (8)
1. a kind of measuring system of single nanoparticle grain size, including a light source, a dark field condenser module, an objective table, one
Object lens, a convex lens, a CCD and its controller, a data line and a display and processing unit are arranged at intervals successively, feature
It is, the monochromatic light that the light source is sent out becomes hollow light cone after dark field condenser module shaping, is irradiated on objective table
And scattering light is generated, scattering light is finally imaged on CCD and its controller by object lens, convex lens, and passes through data line transfer
To display and processing unit, it is corresponding to obtain each nano particle for handling image for the display and processing unit
The strength information of hot spot is scattered, the database in display and processing unit obtains corresponding to each dissipate in details in a play not acted out on stage, but told through dialogues micro-image
Penetrate the grain size of hot spot.
2. the measuring system of single nanoparticle grain size as described in claim 1, which is characterized in that the light of the light source outgoing
For monochromatic light.
3. the measuring system of single nanoparticle grain size as described in claim 1, which is characterized in that the dark field condenser mould
Group includes a diaphragm and a condenser and is set gradually along the light path being emitted from light source.
4. the measuring system of single nanoparticle grain size as claimed in claim 3, which is characterized in that the diaphragm is a diameter of
The round copper sheet of 21mm, the numerical aperture of the condenser is 0.9.
5. the measuring system of single nanoparticle grain size as described in claim 1, which is characterized in that the objective table includes one
Substrate is to carry nanoparticle sample.
6. the measuring system of single nanoparticle grain size as described in claim 1, which is characterized in that the magnifying power of the object lens
It is 100 times, numerical aperture 0.8.
7. the measuring system of single nanoparticle grain size as described in claim 1, which is characterized in that the convex lens is by object lens
The scattering light for the nano particle being collected into is imaged on CCD and its controller, and the details in a play not acted out on stage, but told through dialogues for obtaining the scattering hot spot of nano particle is shown
Micro- image.
8. the measuring system of single nanoparticle grain size as described in claim 1, which is characterized in that the dark field condenser mould
Group is a dark field condenser, and the dark field condenser is parabolic concentrator, in cardioid condenser, concentric spherical condenser
It is a kind of.
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