CN110455690A - Nano particle diameter measuring system - Google Patents
Nano particle diameter measuring system Download PDFInfo
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- CN110455690A CN110455690A CN201910773638.1A CN201910773638A CN110455690A CN 110455690 A CN110455690 A CN 110455690A CN 201910773638 A CN201910773638 A CN 201910773638A CN 110455690 A CN110455690 A CN 110455690A
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- 239000000523 sample Substances 0.000 claims description 88
- 230000003287 optical effect Effects 0.000 claims description 36
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- 239000007788 liquid Substances 0.000 claims description 13
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- 239000011521 glass Substances 0.000 description 4
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- 239000002245 particle Substances 0.000 description 3
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 2
- 240000002853 Nelumbo nucifera Species 0.000 description 2
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 2
- 238000005311 autocorrelation function Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
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- 238000002296 dynamic light scattering Methods 0.000 description 2
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means
- G01N15/0211—Investigating a scatter or diffraction pattern
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means
- G01N15/0211—Investigating a scatter or diffraction pattern
- G01N2015/0222—Investigating a scatter or diffraction pattern from dynamic light scattering, e.g. photon correlation spectroscopy
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- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The application provides a kind of nano particle diameter measuring system.The first smooth blocking-up structure and the second smooth blocking-up structure are placed in matching fluid.First photoresist breaks structure setting on incident beam forward direction extended line, to absorb and the reflected beams, reach it can not and reflects at match-pool wall surface and air interface.Second photoresist break structure setting in it is multiple scattering the received scattered beams of light through-hole reverse extending lines on, for absorbs with reflection measurement acceptance angle supplementary angles on scattered beam, reach it can not and reflected at match-pool wall surface and air interface.The influence of sample cell wall surface reflected light in Conventional nano grain diameter measuring system can be largely reduced by matching fluid, the first smooth blocking-up structure and the second smooth blocking-up structure, and avoid being mixed into reflected light information in multiple scattered light signals for scattering light through-holes reception self-views, so that the accuracy of measurement result greatly improved.
Description
Technical field
This application involves field of measuring technique more particularly to a kind of nano particle diameter measuring systems.
Background technique
The granulometry of nano particle is mainly had electron microscope and is developed a variety of dynamic based on dynamic light scattering theory
State light scatters nano particles measurement method, unordered by a large amount of fluid molecules in periphery when nano particle suspends in a liquid
It hits, random movement can be generated, this movement of particle is known as Brownian movement.Nano particle does Brownian movement in a liquid
When, the scattering light of nano particle can pulse.Since the height of ripple frequency and the diffusion coefficient of nano particle are related, and
Diffusion coefficient is related with the granule size of nano particle, therefore the grain of nano particle can be measured using dynamic light scattering method
Diameter.
But incident beam is scattered that the light beam behind center can be in close Jie of light in traditional nano particle diameter measuring system
It reflects, i.e., is reflected at sample cell wall surface and Air Interface during matter to optically thinner medium.Light beam after reflection can be anti-
The scattering optical receiver apparatus for penetrating direction receives, and causes to scatter in the scattered light signal for the self-view that optical receiver apparatus receives and mix
Enter reflected light information, bring measurement error, so that the measurement result inaccuracy of Conventional nano grain diameter measuring system.
Summary of the invention
Based on this, it is necessary to for the problem of the measurement result inaccuracy of Conventional nano grain diameter measuring system, provide
A kind of nano particle diameter measuring system.
It includes scattering generating device, match-pool, sample cell, matching that the application, which provides a kind of nano particle diameter measuring system,
The disconnected structural support of liquid, end cap, the first photoresist, the first smooth blocking-up structure and the second smooth blocking-up structure.The scattering fills
Set the scattering for making nano particle to be measured that all angles occur under interaction.The scattering generating device includes first
Annular side plate.The first annular side plate surrounds to form first storage space with the first opening.It is described first annular
Side plate is provided with incident light through-hole and multiple scattering light through-holes.The incident light through-hole is set to the multiple scattering light through-hole
Same level.And the axis of the axis of the incident light through-hole and the multiple scattering light through-hole intersects at same scattering center
Point.
The match-pool is set in first storage space.The match-pool includes forming one to have the second opening
The second storage space.The sample cell is set in second storage space, to place sample solution.Incident beam is logical
It crosses after the incident light through-hole exposes to the sample cell and forms scattered beam.The multiple scattering light through-hole is used so that scattering
Light beam passes through.The matching fluid is set in second storage space, and the sample cell is surrounded.And the matching fluid
Refractive index is identical as the refractive index of the sample cell wall surface.The end cap matches setting with first opening.And the end cap
It is provided with the first putting hole.The diameter of the sample cell is less than the diameter of first putting hole.The first smooth blocking-up structure
Support portion is set between the sample cell and the match-pool.The disconnected structural support of first photoresist and the end cap connect
It connects.The first smooth blocking-up structure is used to absorbing and reflecting the light beam after the sample cell.The first smooth blocking-up structure is set
It is placed between the sample cell and the match-pool.The first smooth blocking-up structure and the disconnected structural support of first photoresist connect
It connects.And first photoresist breaks structure setting on incident beam forward direction extended line.Second photoresist breaks structure setting in institute
It states between sample cell and the match-pool.The second smooth blocking-up structure is connect with the end cap.And the disconnected knot of second photoresist
Structure is set on the reverse extending line of the multiple scattering received scattered beam of light through-hole.
In one embodiment, the disconnected structure setting of second photoresist has through-hole.The through-hole, the incident light through-hole with
And the axis of the multiple scattering light through-hole intersects at same scattering center point.The through-bore axis and the incident light through-hole axis
Line is 90 ° in the angle of scattering center point.
In one embodiment, the nano particle diameter measuring system further includes incident electro-optical device.The incident light dress
It sets and the scattering generating device is entered by the incident light through-hole for adjusting incident beam.The incidence electro-optical device includes the
One glan thompson prism and the first prism adjustment structure.First glan thompson prism is set to first prism
Adjustment structure adjusts the position of first glan thompson prism by the first prism adjustment structure, so that incident light
Beam is incident to the incident light through-hole by first glan thompson prism.
In one embodiment, the nano particle diameter measuring system further includes multiple scattering optical receiver apparatuses.Each
The corresponding scattering light through-hole of the scattering optical receiver apparatus, the scattering light issued for receiving the scattering light through-hole
Beam.The receiving light path of the multiple scattering optical receiver apparatus intersects at the same scattering center point of the sample cell.
In one embodiment, each scattering optical receiver apparatus includes reflecting mirror, optical fiber amasthenic lens and optical fiber.
The corresponding scattering light through-hole of one reflecting mirror.The reflecting mirror is set to the scattering that the scattering light through-hole issues
In beam path, for so that scattered beam is reflected with 45 ° of incidence angle.The optical fiber amasthenic lens is set to through described anti-
In scattered beam optical path after penetrating mirror reflection, for being focused to scattered beam.The optical fiber and the optical fiber amasthenic lens
Connection, for the received scattered beam of optical fiber amasthenic lens to be transmitted through the fiber to photon counter.
In one embodiment, each scattering optical receiver apparatus further includes the second glan thompson prism and the second rib
Mirror adjustment structure.Second glan thompson prism is set to the second prism adjustment structure.Pass through second prism
Adjustment structure adjusts the position of second glan thompson prism, so that scattered beam passes through the second Glan Thomson
Prism incidence is to the reflecting mirror.
In one embodiment, the nano particle diameter measuring system further includes charge-coupled device camera.The electricity
Lotus couple device camera is oppositely arranged with first putting hole, for recording incident beam and scattered beam in real time in the sample
The image information of the scattering center point convergence in product pond.
In one embodiment, the nano particle diameter measuring system further includes multiple third putting holes.It is the multiple
Third putting hole is set to the end cap, for placing temperature sensor, with the temperature in the second storage space described in real-time monitoring
Degree.
In one embodiment, the nano particle diameter measuring system further includes temperature control control module and multiple temperature controls
Structure.The temperature control control module is connect with the temperature sensor, for obtaining the temperature in second storage space.Institute
State the outer wall that multiple structure of controlling temperature are set to the first annular side plate far from first storage space, and the multiple temperature
Control structure is connect with the temperature control control module.The temperature control control module becomes according to the temperature in second storage space
Change, regulate and control the multiple structure of controlling temperature, for so that the temperature in second storage space is stablized.
In one embodiment, the end cap is provided with multiple second putting holes, for placing matching liquid pipeline to convey
The matching fluid.
The application provides a kind of above-mentioned nano particle diameter measuring system.The sample cell, the matching fluid, described first
Light blocking-up structure and the second smooth blocking-up structure are all set in the match-pool and surround second storage space to be formed
It is interior.At this point, incident beam is incident to the sample cell by the matching fluid by the incident light through-hole.Incident beam is through dissipating
Enter in the matching fluid after hitting the heart by the pool wall of the sample cell.The scattered beam Jing Guo scattering center is described at this time
Matching fluid Propagation.
The refractive index close of the refractive index of the matching fluid and the sample cell wall surface.The matching fluid can be and glass
The decahydronaphthalene of wall surface refractive index close, it is believed that scattered beam after the sample cell wall surface still with glass wall
The Propagation of face refractive index close.At this point, eliminating the influence of the sample cell wall surface by the matching fluid.
The described first smooth blocking-up structure and the second smooth blocking-up structure are placed in the matching fluid.First light
Blocking-up structure is set on incident beam forward direction extended line, i.e., the described first smooth blocking-up structure is to absorb and reflect at described
With the light beam (incident light is scattered the light beam behind center) propagated in liquid medium, make light beam can not reach the match-pool wall surface with
It is reflected at air interface.At this point, the first smooth blocking-up structure (has already passed through in scattering for the photoresist after 0 ° of incidence is disconnected
The heart).Second photoresist breaks structure setting on the reverse extending line of the multiple scattering received scattered beam of light through-hole.Institute
The reverse extending line for stating multiple scattering received scattered beams of light through-hole is the complementary angular direction for measuring acceptance angle.Second light
Blocking-up structure is used to absorb and reflect the scattered beam on the measurement acceptance angle supplementary angles of the matching fluid Propagation, makes
Scattered beam on supplementary angles can not reach to be reflected at the match-pool wall surface and air interface.
It therefore, can be very big by the matching fluid, the first smooth blocking-up structure and the second smooth blocking-up structure
The influence of sample cell wall surface reflected light in Conventional nano grain diameter measuring system is reduced in degree.Meanwhile passing through the matching
Liquid, the first smooth blocking-up structure and the second smooth blocking-up structure can receive itself to avoid the multiple scattering light through-hole
It is mixed into reflected light information in the scattered light signal of angle, to improve the nano particle diameter measuring system measurement result
Accuracy.
Detailed description of the invention
Fig. 1 is the overall structure diagram of nano particle diameter measuring system provided by the present application；
Fig. 2 is the schematic diagram of the section structure one of scattering generating device provided by the present application；
Fig. 3 is the schematic diagram of the section structure two of scattering generating device provided by the present application；
Fig. 4 is the schematic diagram of the section structure three of scattering generating device provided by the present application；
Fig. 5 is the schematic diagram of the section structure four of scattering generating device provided by the present application；
Fig. 6 is light path schematic diagram in scattering generating device provided by the present application；
Fig. 7 is the schematic diagram of the section structure five of scattering generating device provided by the present application；
Fig. 8 is the overall structure diagram one of scattering generating device provided by the present application；
Fig. 9 is the overall structure diagram two of scattering generating device provided by the present application；
Figure 10 is the overall structure diagram of incident electro-optical device provided by the present application；
Figure 11 is the overall structure diagram of scattering optical receiver apparatus provided by the present application；
Figure 12 is the structural schematic diagram of charge-coupled device camera provided by the present application；
Figure 13 is the overall structure diagram of nano particle diameter measuring instrument provided by the present application.
Description of symbols
Nano particle diameter measuring system 100, scattering generating device 10, match-pool 150, sample cell 180, matching fluid
153, end cap 140, the first photoresist break structural support 161, the first smooth blocking-up structure 160, the second smooth blocking-up structure 170,
First annular side plate 130, first be open the 131, first storage space 132, incident light through-hole 110, scattering light through-hole 120,
Second the 151, second storage space 152 of opening, through-hole 171, incident electro-optical device 20, the first glan thompson prism 210,
First prism adjustment structure 220, scattering optical receiver apparatus 30, reflecting mirror 310, optical fiber amasthenic lens 320, optical fiber 330,
Be isolated plate hole 340, the second glan thompson prism 350, the second prism adjustment structure 360, charge-coupled device camera 40,
Camera tripod 410, structure of controlling temperature 190, temperature control control module 191, laser 50, attenuator 60, the second putting hole
142, sample stage 181, support rod 162, incident aperture 111, the first reflecting mirror 710, the second reflecting mirror 720, lens
730, heat exchanger 80, support base 810, photomultiplier tube 820, correlator 830, nano particle diameter measuring instrument 200,
Tool housing 90, instrument accommodation space 910.
Specific embodiment
In order to which the objects, technical solutions and advantages of the application are more clearly understood, by the following examples, and combine attached
Figure, is further elaborated the application.It should be appreciated that specific embodiment described herein is only to explain this Shen
Please, it is not used to limit the application.
It is herein component institute serialization number itself, such as " first ", " second " etc., is only used for distinguishing described object,
Without any sequence or art-recognized meanings.And " connection ", " connection " described in the application, unless otherwise instructed, include directly and
It is indirectly connected with (connection).In the description of the present application, it is to be understood that term " on ", "lower", "front", "rear", " left side ",
The orientation of the instructions such as " right side ", "vertical", "horizontal", "top", "bottom", "inner", "outside", " clockwise ", " counterclockwise " or position are closed
System indicates to be based on the orientation or positional relationship shown in the drawings, being merely for convenience of description the application and simplifying description
Or imply that signified device or element must have a particular orientation, be constructed and operated in a specific orientation, therefore cannot understand
For the limitation to the application.
In this application unless specifically defined or limited otherwise, fisrt feature in the second feature " on " or " down " can be with
It is that the first and second features directly contact or the first and second features pass through intermediary mediate contact.Moreover, fisrt feature exists
Second feature " on ", " top " and " above " but fisrt feature be directly above or diagonally above the second feature, or be merely representative of
First feature horizontal height is higher than second feature.Fisrt feature can be under the second feature " below ", " below " and " below "
One feature is directly under or diagonally below the second feature, or is merely representative of first feature horizontal height less than second feature.
Referring to Figure 1-9, it includes scattering generating device 10 that the application, which provides a kind of nano particle diameter measuring system 100,.
The scattering generating device 10 includes match-pool 150, sample cell 180, matching fluid 153, end cap 140, the first smooth blocking-up structure branch
Support part 161, the first smooth blocking-up structure 160 and the second smooth blocking-up structure 170.In the sample of the scattering generating device 10
In pond 180, the scattering of all angles occurs under interaction for the nano particle in sample solution.The scattering generating device 10
Including first annular side plate 130.The first annular side plate 130 surrounds first formed one with the first opening 131 and stores
Space 132.The first annular side plate 130 is provided with incident light through-hole 110 and multiple scattering light through-holes 120.The incident light
Through-hole 110 and the multiple scattering light through-hole 120 are set to same level.And axis and the institute of the incident light through-hole 110
The axis for stating multiple scattering light through-holes 120 intersects at same scattering center point.
The match-pool 150 is set in first storage space 132.The match-pool 150 includes forming a tool
There is the second storage space 152 of the second opening 151.The sample cell 180 is set in second storage space 152, to
Place sample solution.Incident beam forms scattered beam after exposing to the sample cell 180 by the incident light through-hole 110.
The multiple scattering light through-hole 120 is used so that scattered beam passes through.The matching fluid 153 is set to second storage space
In 152, and the sample cell 180 is surrounded.And the refraction of the refractive index of the matching fluid 153 and 180 wall surface of sample cell
Rate is identical.The end cap 140 matches setting with first opening 131.And the end cap 140 is provided with the first putting hole 141.
The diameter of the sample cell 180 is less than the diameter of first putting hole 141.The disconnected structural support 161 of first photoresist is set
It is placed between the sample cell 180 and the match-pool 150.The disconnected structural support 161 of first photoresist and the end cap 140
Connection.The first smooth blocking-up structure 160 is used to absorbing and reflecting the light beam after the sample cell 180.First photoresist
Disconnected structure 160 is set between the sample cell 180 and the match-pool 150.The first smooth blocking-up structure 160 and described the
The disconnected structural support 161 of one photoresist connects.And the first smooth blocking-up structure 160 is set on incident beam forward direction extended line.
The second smooth blocking-up structure 170 is set between the sample cell 180 and the match-pool 150.The disconnected knot of second photoresist
Structure 170 is connect with the end cap 140.And the second smooth blocking-up structure 170 is set to the multiple scattering light through-hole 120 and receives
Scattered beam reverse extending line on.
The disconnected knot of the sample cell 180, the matching fluid 153, the first smooth blocking-up structure 160 and second photoresist
Structure 170 is all set in the match-pool 150 and surrounds in second storage space 152 formed.At this point, incident beam passes through institute
It states incident light through-hole 110 and is incident to the sample cell 180 by the matching fluid 153.Incident beam be scattered behind center by
The pool wall of the sample cell 180 enters in the matching fluid 153.The light beam Jing Guo scattering center is in the matching liquid medium at this time
Middle propagation.
The refractive index close of the refractive index of the matching fluid 153 and 180 wall surface of sample cell.The matching fluid 153 can
Think the decahydronaphthalene with glass wall refractive index close, it is believed that the light beam after 180 wall surface of sample cell is still
In the Propagation with glass wall refractive index close.At this point, eliminating the sample cell by the matching fluid 153
The influence of 180 wall surfaces.
The described first smooth blocking-up structure 160 and the second smooth blocking-up structure 170 are placed in the matching fluid 153.
The first smooth blocking-up structure 160 is set on incident beam forward direction extended line, i.e., described first smooth blocking-up structure 160 is to inhale
The light beam (light beam after being scattered center) in 153 Propagation of matching fluid is received and reflected, makes light beam that can not reach institute
It states and is reflected at 150 wall surface of match-pool and air interface.At this point, the first smooth blocking-up structure 160 is the light after 0 ° of incidence
It blocks (having already passed through scattering center).It is received that the second smooth blocking-up structure 170 is set to the multiple scattering light through-hole 120
On the reverse extending line of scattered beam.The reverse extending line of the multiple scattering received scattered beam of light through-hole 120 is measurement
The complementary angular direction of acceptance angle.The second smooth blocking-up structure 170 passes in 153 medium of matching fluid for absorbing and reflecting
The scattered beam on measurement acceptance angle supplementary angles broadcast, makes the scattered beam on supplementary angles that can not reach 150 wall of match-pool
It is reflected at face and air interface.
Therefore, pass through the matching fluid 153, the first smooth blocking-up structure 160 and the second smooth blocking-up structure 170
The influence of sample cell wall surface reflected light in Conventional nano grain diameter measuring system can largely be reduced.Meanwhile passing through
The matching fluid 153, the first smooth blocking-up structure 160 and the second smooth blocking-up structure 170 can be to avoid the multiple
It is mixed into reflected light information in the scattered light signal of the scattering reception self-view of light through-hole 120, to improve the nano particle
The accuracy of 100 measurement result of grain diameter measurement system.
In one embodiment, the axis phase of the axis of the incident light through-hole 110 and the multiple scattering light through-hole 120
Meet at same scattering center point.The incident light through-hole 110 is set to same level with the multiple scattering light through-hole 120,
Incident light and scattering light are intersected at same central point.The nano particle diameter measuring system 100 is in multiple angles
The same scattering center of nano particle to be measured is carried out while being measured, the particle scattering rule from same scattering center can be obtained
Rule, multiangular measurement analysis is more accurate, so that the sampling time of the nano particle diameter measuring system 100 is short, improves
Measurement accuracy.
In one embodiment, the disconnected structural support 161 of first photoresist is detachably connected with the end cap 140.Institute
It states the first photoresist and breaks structural support 161 to the fixed support first smooth blocking-up structure 160.The second smooth blocking-up structure
170 are detachably connected with the end cap 140.The nano particle diameter measuring system 100 further includes sample stage 181, the sample
Sample platform 181 is set in second storage space 152.
The sample stage 181 is provided with sample cell groove close to described 180 one end of sample cell, to place the sample cell
180.Pass through the fixed sample cell 180 of the sample stage 181 support.The nano particle diameter measuring system 100 further includes
The support rod 162 of setting corresponding with the disconnected structural support 161 of first photoresist, the support rod 162 are detachably set to
The end cap 140.The support rod 162 is provided with incident aperture 111.At this point, incident light passes through incident light through-hole 110, enters
It penetrates light aperture 111 and exposes to the sample cell 180.Meanwhile the sample stage 181, the sample cell 180 and the matching
Pond 150 is coaxially disposed, it is ensured that the scattered signal that multi-angle is collected comes from same scattering center.
Fig. 6 is referred to, in one embodiment, the second smooth blocking-up structure 170 is provided with through-hole 171.The through-hole
171, the axis of the incident light through-hole 110 and the multiple scattering light through-hole 120 intersects at same scattering center point.It is described
171 axis of through-hole is 90 ° in the angle of scattering center point with 110 axis of incident light through-hole.
When measuring acceptance angle is 90 °, 90 ° of corresponding 120 axis of scattering light through-hole and the incident light through-hole 110
Axis is 90 ° in the angle of scattering center point.At this point, supplementary angles when measurement acceptance angle is 90 ° remain as 90 °, measurement is received
Scattered beam on the supplementary angles of angle has influence for 100 measurement result of nano particle diameter measuring system.Therefore, pass through
The through-hole 171 is set on the described second smooth blocking-up structure 170, is 90 ° of directions to receive measurement acceptance angle supplementary angles
Scattered beam, to ensure the accuracy of 100 measurement result of nano particle diameter measuring system.
Fig. 8 is referred to, in one embodiment, the end cap 140 is provided with multiple second putting holes 142, for placing
Liquid pipeline is matched to convey the matching fluid 153.
The number of the multiple second putting hole 142 can be 2.Wherein, second putting hole 142 is for putting
Matching liquid pipeline is set, the matching fluid 153 is inputted in Xiang Suoshu match-pool 150.Wherein, another described second putting hole 142
Liquid pipeline is matched for placing, so that the matching fluid 153 exports the match-pool 150.At this point, being put by the multiple second
Hole 142, matching liquid pipeline are set, 153 circulation conveying of matching fluid can be made, described in facilitating in the match-pool 150
Matching fluid 153 updates.
Referring to Figure 10, in one embodiment, the nano particle diameter measuring system 100 further includes incident electro-optical device
20.The incidence electro-optical device 20 enters the scattering generating device by the incident light through-hole 110 for adjusting incident beam
10.The incidence electro-optical device 20 includes the first glan thompson prism 210 and the first prism adjustment structure 220.Described first
Glan thompson prism 210 is set to the first prism adjustment structure 220.It is adjusted by the first prism adjustment structure 220
The position of first glan thompson prism 210 is saved, so that incident beam passes through first glan thompson prism 210
It is incident to the incident light through-hole 110.
The first prism adjustment structure 220 includes support base 221, regulating platform 222 and adjustment axis 223.Regulating platform 222
It is set on support base 221, adjustment axis 223 is slidably connected with regulating platform 222.First glan thompson prism 210 is arranged
In on the regulating platform of the first prism adjustment structure 220, the position of platform 222 is controlled to adjust by adjustment axis 223, so that incident
Light beam is incident to the incident light through-hole 110 by first glan thompson prism 210.Wherein, the first Glan soup
The inferior prism 210 (Glan-Thompson) of nurse is placed in input path, to obtain the polarized incident light of vertical direction, at this time
Incident beam forms the polarized incident light of vertical direction after first glan thompson prism 210, be incident to it is described enter
Penetrate light through-hole 110.
Lens 730 are provided between the incidence electro-optical device 20 and the scattering generating device 10.The lens 730 will hang down
Histogram to polarized incident light focus, by the incident light through-hole 110 be incident to it is described scattering generating device 10 the sample
Product pond 180.
Referring to Figure 1, in one embodiment, the nano particle diameter measuring system 100 further include laser 50 with
And attenuator 60.The laser 50 is for issuing incident beam.The attenuator 60 be set to the incident electro-optical device 20 with
Between the laser 50.The incident beam that the attenuator 60 issues the laser 50 is adjusted, through the decaying
Incident beam after device 60 is adjusted is incident to the incident light through-hole 110 through the incident electro-optical device 20.
Wherein, the laser 50 is high-power H e-Ne laser.The attenuator 60 is attenuator, and function may be implemented
Rate is adjustable.
The nano particle diameter measuring system 100 further includes the first reflecting mirror 710 and the first reflecting mirror 720.Described
One reflecting mirror 710 can be used for adjusting the direction for the incident light that the laser 50 issues.It is adjusted through first reflecting mirror 710
Incident light afterwards realizes the effect of power adjustable by the attenuator 60.First reflecting mirror 720 can be used for adjusting warp
The direction of the incident light of the attenuator 60.Incident light beam strikes after first reflecting mirror 720 adjusting are to the incident light
Device 20.
In one embodiment, the nano particle diameter measuring system 100 further includes multiple scattering optical receiver apparatuses 30.
The multiple scattering optical receiver apparatus 30 collects the scattered light signal issued from scattering center.Each scattering optical receiver apparatus
The 30 corresponding scattering light through-holes 120, the scattered beam issued for receiving the scattering light through-hole 120.It is the multiple
The receiving light path of scattering optical receiver apparatus 30 intersects at the same scattering center point of the sample cell 180.The one scattering light connects
Receiving apparatus 30 corresponds to scattering light through-hole 120, is scattered for receiving from different perspectives containing nanoparticles solution
Scatter light.
Referring to Figure 11, in one embodiment, each scattering optical receiver apparatus 30 includes reflecting mirror 310, optical fiber
Amasthenic lens 320 and optical fiber 330.The corresponding scattering light through-hole 120 of one reflecting mirror 310.The reflecting mirror
310 are set in the scattered beam optical path that the scattering light through-hole 120 issues, be used for so that scattered beam with 45 ° of incidence angle into
Row reflection.The optical fiber amasthenic lens 320 be set to through the reflecting mirror 310 reflection after scattered beam optical path on, for pair
Scattered beam is focused.The optical fiber 330 is connect with the optical fiber amasthenic lens 320, is used for the optical fiber amasthenic lens
320 received scattered beams are transmitted through the fiber to photon counter.
Receive what the scattering light through-hole 120 issued by the optical fiber amasthenic lens 320 and the combination of the optical fiber 330
Scattered beam.While meeting spatial coherence requirement, the light passing amount and use of the scattering optical receiver apparatus 30 are increased
Convenience.Meanwhile the optical fiber amasthenic lens 320 has the function of focusing, and substantially increases the light intensity for receiving signal, and energy
Enough focus on 180 center of sample cell.
Also, photomultiplier tube 820 is connect with optical fiber 330 by optical fiber.The light intensity letter obtained by photomultiplier tube 820
Breath is adjusted in real time, so as to reach at the largest light intensity of each receiving angle, to guarantee scattering center registration highest, and really
The receiving light path for protecting the scattering optical receiver apparatus 30 intersects at the same scattering center point of the sample cell 180.
One photomultiplier tube 820 is connect with a scattering optical receiver apparatus 30, to detect light pulse letter
Number power.The correlator 830 is provided with multiple channels, and a channel connects with 820 optical fiber of photomultiplier tube
It connects, to obtain the light intensity auto-correlation function of multiple scattering angles, and realizes signal conversion, transmission and related operation.Finally exist
Nano particle diameter Inversion Calculation is carried out in computer, and then exports grain diameter measurement result.
The correlator 830 can be correlation receiver, using the correlation properties of signal by useful signal from interfering and make an uproar
The tool extracted in sound.The correlator 830 can be digital correlator, calculate light intensity auto-correlation using digital correlator
Function.The scattering light of multiple angles is received by the scattering optical receiver apparatus 30, by the photomultiplier tube 820 by faint letter
Number identify and extract, and enter the correlator 830, obtain institute's measuring angle at light intensity auto-correlation function.By the phase
Device 830 is closed to connect with computer.Computer and related software are used for according to the scattering light received, the light intensity being recorded at any time
The particle diameter distribution of nano particle in nano granule suspension to be measured is calculated in change information.Carry out nano particle diameter
Inversion Calculation obtains the smallest weight coefficient ratio of error, and exports grain diameter measurement result.
In one embodiment, each scattering optical receiver apparatus 30 further include the second glan thompson prism 350 with
Second prism adjustment structure 360.Second glan thompson prism 350 is set to the second prism adjustment structure 360.It is logical
The position that the second prism adjustment structure 360 adjusts second glan thompson prism 350 is crossed, so that scattered beam passes through
It crosses second glan thompson prism 350 and is incident to the reflecting mirror 310.
The second prism adjustment structure 360 is identical as the structure of the first prism adjustment structure 220.
The second prism adjustment structure 360 includes support base, regulating platform and adjustment axis.Regulating platform is set to support base
On, adjustment axis is slidably connected with regulating platform.Second glan thompson prism 350 is set to the second prism adjustment structure
On 360 regulating platform, the position of regulating platform is set by adjustment axis, so that emergent light (scattered beam) passes through second Glan
Thomson prism 350 exposes on the reflecting mirror 310.The optical fiber amasthenic lens 320 is reflexed to through the reflecting mirror 310.
Specifically, each scattering optical receiver apparatus 30 further includes fixing seat 370.The fixing seat 370 and the branch
Support seat 810 is detachably connected.The reflecting mirror 310, the optical fiber amasthenic lens 320, the optical fiber 330, second Glan
Thomson prism 350 and the second prism adjustment structure 360 are placed in fixing seat 370.Fixing seat 370 includes multiple solid
Fixed board, multiple fixed plates surround and to form the second prism adjustment structure placement space, reflecting mirror places space and optical fiber amasthenic lens
Place space.Reflecting mirror, which places space and optical fiber amasthenic lens and places space, to be arranged in side, and with the second prism adjustment structure
Space is placed to separate by isolation board.Isolation board is provided with isolation plate hole 340.Reflecting mirror places space to place the reflection
Mirror 310.Optical fiber amasthenic lens places space setting and places space above in reflecting mirror, and optical fiber amasthenic lens places space and anti-
It penetrates mirror and places space connection.Second prism adjustment structure places space for placing the second prism adjustment structure 360.Scattering
Light beam is by second glan thompson prism 350 to isolation plate hole 340.Also, it is exposed to by isolation plate hole 340 described
Reflecting mirror 310.Scattered beam reflexes to the optical fiber amasthenic lens 320 through the reflecting mirror 310, forms the light of scattered beam
Road.
Wherein, when testing the rod-like nanoparticles partial size of a certain measurement receiving angle, the second Glan Thomson rib
Mirror 350 (Glan-Thompson) is placed on scattered beam receiving light path, to filter out the orthogonal polarized light in scattered signal.
At this point, scattered beam exposes to the reflecting mirror 310 through plate hole 340 is isolated after second glan thompson prism 350.
When testing the spherical nanoparticles partial size of a certain measurement receiving angle, second glan thompson prism 350
(Glan-Thompson) it removes.
Referring to Figure 1, in one embodiment, the nano particle diameter measuring system 100 further includes charge-coupled device
Part camera 40.The charge-coupled device camera 40 is oppositely arranged with first putting hole 141, for recording incident light in real time
The image information that beam and scattered beam are converged in the scattering center point of the sample cell 180.
Wherein, first putting hole 141 corresponds to the opening of the sample cell 180.The charge-coupled device camera
40 and the opening of the sample cell 180 be oppositely arranged.Also, the charge-coupled device camera 40 is communicated to connect with computer end,
To transmit the 40 acquired image information of charge-coupled device camera.The charge-coupled device camera 40 faces institute
The opening of sample cell 180 is stated, display incident light and emergent light (scattered beam) can be recorded in real time at 180 center of sample cell
The image information of convergence.Also, the effect focused by the charge-coupled device camera 40 can be observed intuitively multiple described
Whether the scattering light-receiving optical path of scattering optical receiver apparatus 30 strictly intersects at the same scattering center point of the sample cell 180,
The fine tuning of spatial triaxial coordinate can be carried out to realize truly concentric.It can be with by the charge-coupled device camera 40
Observation calculates the measurement angle of scattering light-receiving light, it is ensured that the accuracy of each scattering light-receiving angle.Meanwhile according to described
40 acquired image information of charge-coupled device camera, the angle of adjustable multiple scattering optical receiver apparatuses 30 are come real
The scattering light measurement of existing a certain determining receiving angle.
It therefore, can be with the multiple scattering optical receiver apparatuses 30 of real-time detection by the charge-coupled device camera 40
Receiving angle, and carry out accordingly be adjusted to ensure that it is each scattering light-receiving angle accuracy.To pass through the electricity
Lotus couple device camera 40 can place one's entire reliance upon existing machining accuracy no longer to guarantee multiple scattering light-receiving optical path intersections
In the precision of the same scattering center point of the sample cell 180.
In one embodiment, the nano particle diameter measuring system 100 further includes instrument fixed plate 840.It is described to dissipate
Penetrate generating device 10, the incident electro-optical device 20, the laser 50, the attenuator 60, first reflecting mirror 710, institute
It states the second reflecting mirror 720, the heat exchanger 80, the photomultiplier tube 820 and the correlator 830 and is detachably arranged at institute
It states in instrument fixed plate 840, connection easy to disassemble, improves the portability and stability of device.The scattering optical receiver apparatus
30, the lens 730 are set on the support base 810, and the support base 810 is detachably arranged at the instrument fixed plate
On 840, connection easy to disassemble improves the portability and stability of device.
It can make all devices in the nano particle diameter measuring system 100 by the instrument fixed plate 840
It integrates, is convenient for carrying movement.The charge-coupled device camera 40 is fixed on described by multiple camera tripods 410
In instrument fixed plate 840.And the surface at the center of the sample cell 180 is arranged in the charge-coupled device camera 40, and
It is connect with computer, to record the scattering center point convergence of incident beam and scattered beam in the sample cell 180 in real time
Image information.
Fig. 8-9 is referred to, in one embodiment, the nano particle diameter measuring system 100 further includes multiple thirds
Putting hole 143.The multiple third putting hole 143 is set to the end cap 140, for placing temperature sensor, to supervise in real time
Survey the temperature in second storage space 152.The nano particle diameter measuring system 100 further includes temperature control control module
191 and multiple structure of controlling temperature 190.The temperature control control module 191 is connect with the temperature sensor, for obtaining described
Temperature in two storage spaces 152.The multiple structure of controlling temperature 190 is set to described far from first storage space 132
The outer wall of first annular side plate 130, and the multiple structure of controlling temperature 190 is connect with the temperature control control module 191.The temperature control
Control module 191 regulates and controls the multiple structure of controlling temperature 190, for making according to the temperature change in second storage space 152
The temperature obtained in second storage space 152 is stablized.
The structure of controlling temperature 190 can be set in the first annular side plate 130 of the opposite sides of the sample cell 180
Outer wall, realize the control of temperature control.Temperature by adjustable second storage space 152 of the structure of controlling temperature 190 is
80 DEG C or so.The structure of controlling temperature 190 can be cooling piece, by connection water pipe to utilize water circulation system to realize the tune of temperature
Control.
The structure of controlling temperature 190 is also connect with temperature control control module 191.When being arranged in the third putting hole 143
When temperature sensor monitors that the temperature in the sample cell 180 and in the match-pool 150 changes, temperature parameter is passed
Transport to the temperature control control module 191.At this point, adjusting the structure of controlling temperature 190 by the temperature control control module 191, realize
Equalized temperature is stablized.
In one embodiment, the structure of controlling temperature 190 is circulating water line, the temperature control control module 191 and circulation
Pump connection.When temperature change in the second storage space 152 described in 191 real-time monitoring of temperature control control module, the temperature
The power of 191 control loop water pump of control module, and then the water flow output of control loop water pump are controlled, realizes the regulation of temperature.
In turn, make the temperature in second storage space 152 be maintained at 80 DEG C or so by heat transfer, be the sample cell
180 provide stable environment, improve the measurement accuracy of the nano particle diameter measuring system 100.
In one embodiment, there are two the third putting holes 143 for the setting of end cap 140.One third is put
It sets and places a temperature sensor in hole 143, a temperature sensor is placed in the sample cell 180, described for monitoring
Temperature in sample cell 180.A temperature sensor is placed in another described third putting hole 143, temperature sensor is placed
In in second storage space 152 of the match-pool 150, for monitoring the temperature in the match-pool 150.The temperature control
Control module 191 monitors the temperature change in the sample cell 180 and second storage space 152 simultaneously.When the temperature control
When the temperature that control module 191 monitors the sample cell 180 changes, the temperature control control module 191 passes through the temperature control
Structure 190 is adjusted, and then makes the temperature in second storage space 152 be maintained at 80 DEG C or so by heat transfer, and
So that the temperature in the sample cell 180 is maintained at 80 DEG C or so, stable environment is provided.
Therefore, by between the structure of controlling temperature 190, the first annular side plate 130, the match-pool 150
Heat transmitting, can make the temperature change in the sample cell 180 at each position identical on the whole, realize the sample cell
The synchronous variation of temperature in 180 at each position.At this point, the nano particle in the sample cell 180 does Blang's fortune in a liquid
When dynamic, the influence of temperature factor not will receive, so that nano particle is in a metastable environment.Also, pass through institute
The heat transmitting between structure of controlling temperature 190, the first annular side plate 130, the match-pool 150 is stated, is not in described
The problem of temperature in sample cell 180 is increased suddenly or is reduced suddenly.
In one embodiment, the temperature control control module 191 includes but is not limited to central processing unit (Center
Processor Unit, CPU), embedded microcontroller (Micro Controller Unit, MCU), embedded microprocessor
(Micro Processor Unit, MPU), Embedded SoC (System on Chip, SoC).
Referring to Figure 13, in one embodiment, a kind of nano particle diameter measuring instrument 200 includes tool housing 90.
The tool housing 90, which surrounds, forms an instrument accommodation space 910.The nano particle diameter measuring system 100 is placed in institute
It states in instrument accommodation space 910, to provide closing no light conditions for the nano particle diameter measuring system 100, prevents it
His stray light.
Wherein, the heat exchanger 80 is set to the instrument fixed plate 840, to maintain the instrument accommodation space 910
Interior environment temperature it is constant.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The several embodiments of the application above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
The limitation to the application the scope of the patents therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the concept of this application, various modifications and improvements can be made, these belong to the guarantor of the application
Protect range.Therefore, the scope of protection shall be subject to the appended claims for the application patent.
Claims (10)
1. a kind of nano particle diameter measuring system characterized by comprising
It scatters generating device (10), for so that the scattering of all angles occurs under interaction for nano particle to be measured；
The scattering generating device (10) includes first annular side plate (130), and the first annular side plate (130), which is surrounded, forms one
A first storage space (132) with the first opening (131), the first annular side plate (130) are provided with incident light through-hole
(110) it is set to multiple scattering light through-holes (120), the incident light through-hole (110) with the multiple scattering light through-hole (120)
Same level, and the axis of the incident light through-hole (110) and the axis of the multiple scattering light through-hole (120) intersect at together
Scattering center point；
Match-pool (150) is set in first storage space (132), and the match-pool (150) includes forming one to have
The second storage space (152) of second opening (151)；
Sample cell (180) is set in second storage space (152), and to place sample solution, incident beam passes through institute
It states incident light through-hole (110) and exposes to the sample cell (180) by scattering center formation scattered beam, the multiple scattering light
Through-hole (120) is used so that scattered beam passes through；
Matching fluid (153) is set in second storage space (152), and the sample cell (180) is surrounded, and described
The refractive index of matching fluid (153) is identical as the refractive index of the sample cell (180) wall surface；
End cap (140) matches setting with first opening (131), and the end cap (140) is provided with the first putting hole
(141), the diameter of the sample cell (180) is less than the diameter of first putting hole (141)；
First photoresist breaks structural support (161), is set between the sample cell (180) and the match-pool (150), and institute
The first photoresist disconnected structural support (161) is stated to connect with the end cap (140)；
First smooth blocking-up structure (160), for absorbing and reflecting the light beam after the sample cell (180), first photoresist
Disconnected structure (160) are set between the sample cell (180) and the match-pool (150), the first smooth blocking-up structure (160)
It is connect with first photoresist disconnected structural support (161), and the first smooth blocking-up structure (160) is being set to incident beam just
To on extended line；
Second smooth blocking-up structure (170), is set between the sample cell (180) and the match-pool (150), second light
Blocking-up structure (170) is connect with the end cap (140), and the second smooth blocking-up structure (170) is set to the multiple scattering
On the reverse extending line of light through-hole (120) received scattered beam.
2. nano particle diameter measuring system as described in claim 1, which is characterized in that the second smooth blocking-up structure
(170) it is provided with through-hole (171), the through-hole (171), the incident light through-hole (110) and the multiple scattering light through-hole
(120) axis intersects at same scattering center point, and through-hole (171) axis and incident light through-hole (110) axis exist
The angle of scattering center point is 90 °.
3. nano particle diameter measuring system as described in claim 1, which is characterized in that further include:
Incident electro-optical device (20) is filled by the incident light through-hole (110) into the scattering for adjusting incident beam
Set (10)；
The incidence electro-optical device (20) includes the first glan thompson prism (210) and the first prism adjustment structure (220), institute
It states the first glan thompson prism (210) and is set to the first prism adjustment structure (220)；
The position of first glan thompson prism (210) is adjusted by the first prism adjustment structure (220), so that
Incident beam is incident to the incident light through-hole (110) by first glan thompson prism (210).
4. nano particle diameter measuring system as described in claim 1, which is characterized in that further include:
Multiple scattering optical receiver apparatuses (30), each corresponding scattering light through-hole of the scattering optical receiver apparatus (30)
(120), the scattered beam issued for receiving scattering light through-hole (120)；
The receiving light path of the multiple scattering optical receiver apparatus (30) intersects at the same scattering center point of the sample cell (180).
5. nano particle diameter measuring system as claimed in claim 4, which is characterized in that each scattering optical receiver apparatus
(30) include:
Reflecting mirror (310), the corresponding scattering light through-hole (120) of a reflecting mirror (310), the reflecting mirror
(310) it is set in the scattered beam optical path that scattering light through-hole (120) issues, is used for so that scattered beam is with incidence angle
45 ° are reflected；
Optical fiber amasthenic lens (320) is set in the scattered beam optical path after the reflecting mirror (310) reflection, for scattered
Irradiating light beam is focused；
Optical fiber (330) is connect with the optical fiber amasthenic lens (320), for the optical fiber amasthenic lens (320) is received scattered
Irradiating light beam is transmitted through the fiber to photon counter.
6. nano particle diameter measuring system as claimed in claim 5, which is characterized in that each scattering optical receiver apparatus
It (30) further include the second glan thompson prism (350) and the second prism adjustment structure (360)；
Second glan thompson prism (350) is set to the second prism adjustment structure (360)；
The position of second glan thompson prism (350) is adjusted by the second prism adjustment structure (360), so that
Scattered beam is incident to the reflecting mirror (310) by second glan thompson prism (350).
7. nano particle diameter measuring system as described in claim 1, which is characterized in that further include:
Charge-coupled device camera (40) is oppositely arranged with first putting hole (141), in real time record incident beam and
The image information that scattered beam is converged in the scattering center point of the sample cell (180).
8. nano particle diameter measuring system as described in claim 1, which is characterized in that further include:
Multiple third putting holes (143), are set to the end cap (140), for placing temperature sensor, described in real-time monitoring
Temperature in second storage space (152).
9. nano particle diameter measuring system as claimed in claim 8, which is characterized in that further include:
Temperature control control module (191), connect with the temperature sensor, for obtaining in second storage space (152)
Temperature；
Multiple structure of controlling temperature (190) are set to the first annular side plate (130) far from first storage space (132)
Outer wall, and the multiple structure of controlling temperature (190) is connect with the temperature control control module (191)；
The temperature control control module (191) regulates and controls the multiple temperature according to the temperature change in second storage space (152)
It controls structure (190), is used for so that the temperature in second storage space (152) is stablized.
10. nano particle diameter measuring system as described in claim 1, which is characterized in that the end cap (140) is provided with more
A second putting hole (142), for placing matching liquid pipeline to convey the matching fluid (153).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910773638.1A CN110455690A (en) | 2019-08-21 | 2019-08-21 | Nano particle diameter measuring system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910773638.1A CN110455690A (en) | 2019-08-21 | 2019-08-21 | Nano particle diameter measuring system |
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| CN108287126A (en) * | 2018-03-23 | 2018-07-17 | 中国计量科学研究院 | Nano particle diameter measuring system |
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| CN201277938Y (en) * | 2008-10-16 | 2009-07-22 | 丹东百特科技有限公司 | Single-beam double-lens laser particle analyzer |
| US20120120388A1 (en) * | 2010-10-29 | 2012-05-17 | Roche Diagnostics Operations, Inc. | System for Performing Scattering and Absorbance Assays |
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