CN107782642A - A kind of multi-peak particle swarm particle diameter distribution detection means - Google Patents

A kind of multi-peak particle swarm particle diameter distribution detection means Download PDF

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Publication number
CN107782642A
CN107782642A CN201710889301.8A CN201710889301A CN107782642A CN 107782642 A CN107782642 A CN 107782642A CN 201710889301 A CN201710889301 A CN 201710889301A CN 107782642 A CN107782642 A CN 107782642A
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China
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photodetector
disk
light
micro
fluidic chip
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CN201710889301.8A
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Chinese (zh)
Inventor
郭文平
余俊慧
李微
杨克成
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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Priority to CN201710889301.8A priority Critical patent/CN107782642A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/02Investigating particle size or size distribution
    • G01N15/0205Investigating particle size or size distribution by optical means, e.g. by light scattering, diffraction, holography or imaging

Abstract

The invention discloses a kind of multi-peak particle swarm particle diameter distribution detection means, belong to field of optical measurements, it includes micro-fluidic chip, miniflow pump, laser, first focus lens group, second focus lens group, disk adjustment frame, photodetector, digital correlator and computer, micro-fluidic chip is arranged in disk adjustment frame, the fluid channel connected with miniflow pump is provided with micro-fluidic chip, photodetector is arranged in disk adjustment frame or periphery, first focus lens group is used to the emergent light of laser is collimated and focused on, second focus lens group is used to the scattering light being emitted from sample cell converging to photodetector, digital correlator is used to obtain the light intensity auto-correlation function at institute's measuring angle according to discrete light subnumber, computer is used for the particle diameter that sample is obtained according to the inverting of light intensity auto-correlation function.Apparatus of the present invention are easily achieved, it is low to consume sample amount, in site measurement can be achieved and the dynamic scattering light to multiple angles measures simultaneously.

Description

A kind of multi-peak particle swarm particle diameter distribution detection means
Technical field
The invention belongs to field of optical measurements, more particularly, to a kind of multi-peak particle swarm based on micro-fluidic chip Particle diameter distribution detection means.
Background technology
In fields such as chemistry, food industry, biology and marine ecologies, for the particle diameter distribution of submicron particles group Research is extremely important.At present, conventional particle size measuring techniques mainly have sedimentation, micro-image method, electric-resistivity method, Sieve method and dynamic light scattering method etc., but limited by operation principle, except the photon phase in microscopic method and dynamic light scattering method Close outside spectroscopic methodology, other methods are generally unsuitable for the measurement to the particle below micron.
Dynamic light scattering technique is the effective ways for measuring sub-micron and nano particle, and it passes through the auto-correlation of scattered light intensity Function obtains grain graininess and its distribution.And the granularity and distribution of sub-micron and nano particle are to characterize the main ginseng of its performance Number, therefore the measurement to these parameters is significant.
The granular system that the dynamic light scattering technique of single angle is distributed to unimodal or narrow peak, which can provide, more accurately to be surveyed Measure result.However, for the granular system of wide distribution, bimodal distribution and multi-modal, single scattering angle dynamic light scattering The grain diameter information that data are included is imperfect, so as to cause the failure of grain diameter inverting.
Therefore, it is necessary to develop a kind of new measuring method or detection means suitable for multi-peak particle swarm particle diameter.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of multi-peak particle swarm particle diameter distribution Detection means, it is intended that by together with photoelectric detector and micro-fluidic chip ingehious design, by being surveyed in multiple angles Amount scattering light obtains the particle diameter of multi-peak particle swarm colony, thus solves inapplicable wide point of the dynamic light scattering technique of single angle The technical problem of the granular system grain diameter measurement of cloth, bimodal distribution and multi-modal.
To achieve the above object, the invention provides a kind of multi-peak particle swarm particle diameter distribution detection means, it includes micro- Fluidic chip, miniflow pump, laser, the first focus lens group, the second focus lens group, disk adjustment frame, photodetector, number Word correlator and computer, wherein,
Micro-fluidic chip is arranged in disk adjustment frame, and the flat as sample cell is provided with the micro-fluidic chip Fluid channel, flat fluid channel connection miniflow pump, miniflow pump are used to the sample of grain diameter to be measured being pumped to flat Fluid channel, photodetector are arranged in disk adjustment frame or are arranged on disk adjustment frame periphery, and the first focus lens group is set Put on laser emitting light direction, for being collimated and being focused on the emergent light of laser, go out from the first focus lens group The laser facula penetrated is incident in the sample cell of micro-fluidic chip, is scattered through the particle in sample cell, the second condenser lens Group is used to the scattering light being emitted from sample cell converging to photodetector, and the photodetector is arranged on the second condenser lens On the outgoing light direction of group, for scattering the number of photons of light, the digital correlation at institute's measuring angle in recruiting unit's time Device is used to be used for foundation light intensity from phase according to the light intensity auto-correlation function at discrete light subnumber acquisition institute measuring angle, the computer Close the particle diameter that function inversion obtains sample.
Further, the disk adjustment frame includes outer disc, inner disk and disk rotary rotating shaft, wherein, it is outer disc, interior Disk is coaxially disposed, and disk rotary rotating shaft is arranged at the common axle center of outer disc and inner disk, outer disc and disk rotary rotating shaft It can be rotated along common axle center, inner disk is fixed.
Further, photodetector has multiple, and micro-fluidic chip is arranged on fixed inner disk axle center and gone out, more Individual photodetector is arranged on the edge of outer disc, can receive the scattering light of multiple angles.
Further, photodetector has three, solid respectively in the outer disc relevant position corresponding to three angle of scatterings Determine photodetector, while measure the dynamic scattering light corresponding to one group of angle of scattering,
Photodetector output light electric current accesses the digital correlator of triple channel, during work, outer disc is rotated, that can obtain The dynamic scattering light of a variety of different angles.
Further, photodetector has one, and a photodetector is arranged on disk adjustment frame upper periphery simultaneously And it is fixed, micro-fluidic chip is arranged in rotatable disk rotary rotating shaft, and during work, rotating circular disc rotary shaft is micro- to rotate Fluidic chip, so as to make photodetector obtain the scattering light of multiple angles.
Further, photodetector has one, and a photodetector is arranged at the maximum annulus of outer disc, Micro-fluidic chip is arranged at the axle center of inner disk and fixed, during work, outer disc is rotated, to adjust photodetector Direction, so as to make photodetector obtain the dynamic scattering light of multiple angles.
Further, the photodetector is photomultiplier or photon counter.
Further, the photon counter is single photon counter, small-signal can be identified and extracted, from Improve the accuracy of Monitoring Data.
The invention discloses the multi-peak particle swarm particle diameter distribution of a kind of combination micro-fluidic chip and dynamic light scattering technique Detection method and device.Main, the beam of coherent light from laser is irradiated to equipped with the micro- of polymeric particles suspension In fluidic chip, the polymeric particles suspension in irradiation fluid channel.The scattering light of multiple angles is received by a photoelectric detector, and Into digital correlator, the light intensity auto-correlation function at institute's measuring angle is obtained, is obtained using computer by suitable inversion algorithm The minimum weight coefficient ratio of error is obtained, the size distribution and theoretical value that inverting obtains are closest.
The present invention combines advantage of the micro-fluidic chip to the accurate control of tested sample, proposes that one kind is easily achieved, consumes sample amount The method that dynamic scattering light of low, the achievable in site measurement simultaneously simultaneously to multiple angles measures, the angle for increasing measurement are Size analysis provides more information, can lift the accuracy and robustness of Size analysis.
In general, by the contemplated above technical scheme of the present invention compared with prior art, it can obtain down and show Beneficial effect:
1st, in apparatus of the present invention, the volume of micro-fluidic chip is small, and the flat microchannel on micro-fluidic chip is designed Into sample cell, scattering volume is dramatically reduced, its scattering volume is on the yardstick of micron level, and such ingenious utilization is micro- Fluidic chip significantly shortens light path, multiple scattering, such structure design is eliminated from scattering mechanism as sample cell Have a clear superiority.
2nd, because micro-fluidic chip volume is small, required sample is few when detection, and sample consumption is low, whole detection The size of device is small, and because the position of photodetector or micro-fluidic chip can rotate, multimetering can be achieved.
Brief description of the drawings
Fig. 1 is the structural representation of multi-peak particle swarm particle diameter distribution detection means in the embodiment of the present invention;
Fig. 2 is the structural representation of multi-peak particle swarm particle diameter distribution detection means in the embodiment of the present invention 1, wherein, light Electric explorer 8 has one, and photodetector 8 is arranged at the maximum annulus of outer disc, and micro-fluidic chip 7 is arranged on inner disk Axle center at and it is fixed;
Fig. 3 is the structural representation of multi-peak particle swarm particle diameter distribution detection means in the embodiment of the present invention 2, wherein, light Electric explorer 8 has one, and photodetector 8 is arranged on disk adjustment frame periphery and fixed, and micro-fluidic chip 7 is set Can rotate in rotatable disk rotary rotating shaft;
Fig. 4 is the structural representation of multi-peak particle swarm particle diameter distribution detection means in the embodiment of the present invention 3, wherein, light Electric explorer 8 has three, and micro-fluidic chip 7 is arranged on the fixed axle center of inner disk 5 and gone out, and multiple photodetectors 8 are set Put in the edge of outer disc, so that the scattering light of multiple angles can be received.
Fig. 5 is the light intensity auto-correlation function curve under 30 °, 45 °, 60 ° of scattering angles in the embodiment of the present invention.
The grain graininess point that Fig. 6 goes out for the light intensity auto-correlation function log inversion under the scattering angle after comprehensive multiple angles Cloth curve map and real particle size distribution curve map.
In all of the figs, identical reference is used for representing identical element or structure, wherein:
1st, laser 2, the first focus lens group 3, disk adjustment frame
4th, outer disc 5, inner disk 6, miniflow pump
7th, micro flow chip 8, photodetector 9, digital correlator
10th, computer 11, suspension 12, particle
13rd, the second focus lens group
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below Conflict can is not formed each other to be mutually combined.
Fig. 1 is the structural representation of multi-peak particle swarm particle diameter distribution detection means in the embodiment of the present invention, as seen from the figure, It includes micro-fluidic chip 7, miniflow pump 6, laser 1, the first focus lens group 2, the second focus lens group 13, disk adjustment frame 3rd, photodetector 8, digital correlator 9 and computer 10.
Wherein, micro-fluidic chip 7 is arranged in disk adjustment frame 3, is provided with the micro-fluidic chip 7 as sample cell Flat fluid channel, flat fluid channel connection miniflow pump 6, miniflow pump 6 is used for the sample pump of grain diameter to be measured Flat fluid channel is delivered to, photodetector 8 is arranged in disk adjustment frame or be arranged on disk adjustment frame periphery, and first is poly- Focus lens group 2 is arranged on laser 1 and is emitted on light direction, for being collimated and being focused on the emergent light of laser 1, from first The laser facula that focus lens group 2 is emitted is incident in the sample cell of micro-fluidic chip 7, occurs to dissipate through the particle in sample cell Penetrate, the second focus lens group 13 is used to the scattering light being emitted from sample cell converging to photodetector 8, the photodetector 8 are arranged on the outgoing light direction of the second focus lens group 13, for scattering light at institute's measuring angle in recruiting unit's time Number of photons, the digital correlator 9 is used to obtain light intensity auto-correlation function at institute measuring angle according to discrete light subnumber, described Computer 10 is used for the particle diameter that sample is obtained according to the inverting of light intensity auto-correlation function.
In Fig. 1, disk adjustment frame is not drawn, the disk adjustment frame 3 includes outer disc 4, inner disk 5 and disk Rotary shaft, wherein, outer disc 4, inner disk 5 are coaxially disposed, and disk rotary rotating shaft is arranged on the common of outer disc 4 and inner disk 5 At axle center, outer disc 4 and disk rotary rotating shaft can rotate along common axle center, and inner disk 5 is fixed.Put into practice in Practical Project In, in disk adjustment frame, inner disk superposition is arranged on outer disc, and inner disk diameter is less than outer disc diameter, and two disks are same Axle is set.Disk rotary rotating shaft is arranged at the axle center of two disks, and it can be outside prominent inner disk or including depression Below disk.When disc rotary aixs cylinder goes out outside lower inner disk, micro-fluidic chip 7 can be arranged on disk rotary in a manner of suspension In rotating shaft.When disk rotary rotating shaft depression is below inner disk, micro-fluidic chip can be directly anchored at inner disk axle center. Disk rotary rotating shaft can be arranged to rise to the form that can either shrink, by Design of Mechanical Structure with according to need Adjust its structure and realize different functions.
Fig. 2 is the structural representation of multi-peak particle swarm particle diameter distribution detection means in the embodiment of the present invention 1, wherein, light Electric explorer 8 has one, and a photodetector 8 is arranged at the maximum annulus of outer disc, and micro-fluidic chip 7 is arranged on It is at the axle center of inner disk and fixed, during work, outer disc is rotated, to adjust photodetector direction, so as to make light Electric explorer 8 obtains the dynamic scattering light of multiple angles.
Fig. 3 is the structural representation of multi-peak particle swarm particle diameter distribution detection means in the embodiment of the present invention 2, wherein, light Electric explorer 8 has one, and a photodetector 8 is arranged on disk adjustment frame upper periphery and fixed, micro-fluidic Chip 7 is arranged in rotatable disk rotary rotating shaft, during work, rotating circular disc rotary shaft to rotate micro-fluidic chip 7, so as to Photodetector 8 is set to obtain the scattering light of multiple angles.
Fig. 4 is the structural representation of multi-peak particle swarm particle diameter distribution detection means in the embodiment of the present invention 3, wherein, light Electric explorer 8 have it is multiple, micro-fluidic chip 7 is arranged on the fixed axle center of inner disk 5 and gone out, and multiple photodetectors 8 are set Put in the edge of outer disc, so that the scattering light of multiple angles can be received.Specifically, photodetector 8 has three, at three Photodetector is fixed in outer disc relevant position corresponding to angle of scattering respectively, while measures the dynamic corresponding to one group of angle of scattering Light is scattered, the output light electric current of photodetector 8 accesses the digital correlator of triple channel, during work, outer disc is rotated, that can obtain The dynamic scattering light of a variety of different angles.
For example, three angle of scatterings are one group, at 30 °, 45 °, 60 ° dispose three photodetectors, photodetector respectively Signal accesses three-channel digital correlator.By cylindrical 0 ° of disc spins, it can detect and obtain 30 °, 45 °, the dynamic scattering corresponding to 60 ° Light.Outer disc is rotated by 90 °, can measure 120 °, 135 °, the dynamic scattering light corresponding to 150 °.
In the present invention, the photodetector is photomultiplier or photon counter.In order to detect faint light Signal, the photon counter are single photon counter, small-signal can be identified and extracted, from improving monitoring number According to accuracy.
In the present invention, can use with good optical characteristic polymeric material PDMS make micro-fluidic chip, i.e., poly- two Methylsiloxane (Polydimethylsiloxane), required fluid channel is processed by photolithographic exposure technique.
The course of work of apparatus of the present invention is:
Beam of coherent light from laser 2 is irradiated in the micro-fluidic chip 7 equipped with the suspension 11 of particle 12, and irradiation is micro- Particle suspension liquid in runner.The scattering light of multiple angles is received by photodetector 8, and enters digital correlator 9, obtains institute Light intensity auto-correlation function at measuring angle, the minimum weight coefficient of error is obtained by suitable inversion algorithm using computer 10 Than the size distribution that inverting obtains is closest in theoretical value.
In apparatus of the present invention, by designing minim channel, reduce scattering volume, shorten light path, eliminated from scattering mechanism Multiple scattering.Its sample consumption is low, size sensor is small, multimetering can be achieved.
The method that the detection of multi-peak particle swarm particle diameter distribution is carried out using apparatus above is comprised the following steps:
S1:The working fluid of the stability of flow comprising candidate particles group is produced using miniflow pump, is sent into micro-fluidic chip, it is micro- Sample cell of the circulation road as candidate particles group;
S2:The light that laser is sent is transferred to the sample cell of micro-fluidic chip, candidate particles after first group of condenser lens Group's liquid sends scattering light;
S3:Scattering light is focused on photodetector target surface by second group of condenser lens, and photodetector produces photoelectricity Stream;
S4:Photoelectric current enters digital correlator, obtains the light intensity auto-correlation function at multiple scattering angles;
S5:Light intensity auto-correlation function is performed data processing, calculates the average grain diameter particle diameter distribution for obtaining candidate particles group Function.
In the embodiment of above method, in step S4, the light intensity auto-correlation function at least three scattering angles is obtained. Rotatable micro-fluidic chip rotates photodetector, to obtain the light intensity auto-correlation function at multiple scattering angles.Dissipating Firing angle θjThe normalized format of the light intensity auto-correlation function detected is:
In formula:
Wherein, j=1,2,3 ... M, β are the spatial coherence factor, θjFor the angle of scattering of j passages, n is the refraction of decentralized medium Rate, λ0For the wavelength of incident light in a vacuum, KBFor Boltzmann constant, T is absolute temperature, and η is the viscosity of decentralized medium, and D is Peak diameter, τjFor the time delay of j passages, M is port number, DTIt is peak diameter under absolute temperature T.
In step S5, using the auto-correlation function of M passage, based on the above-mentioned equation of Phillips-Twomey Algorithm for Solving Group, inverting have the particle swarm particle diameter distribution of multiple particle diameter peak values.Phillips-Twomey algorithms are that inverting obtains particle diameter distribution One of numerous algorithms, can also be obtained using such as recurrent least square method, CONTIN algorithms and Tikhonov regularization algorithms Obtain particle swarm particle diameter distribution., it is necessary to the weight coefficient of each angle of scattering accurately be set, so as to improve multi-peak in algorithm design Particle swarm particle size distribution inversion accuracy.It can realize that weight coefficient is adaptive by the methods of iterative algorithm, neural metwork training It should adjust.
Fig. 5 is the light intensity auto-correlation function curve under 30 °, 45 °, 60 ° of scattering angles in the embodiment of the present invention.In miniflow The right side in road scattering light to multiple angles can detect simultaneously, and the corresponding photodetector of each angle, can will be more The light intensity auto-correlation function of individual different scattering angle measurements is attached in a data analysis.As can be seen from Figure 5,30 °, 45 °, 60 ° Light intensity auto-correlation function curve under scattering angle relatively kissed with preferable auto-correlation function curve ratio and, it is known that, apparatus of the present invention Design is feasible.
The accuracy of measuring method is examined using the aqueous solution of polystyrene standard spheric granules.Laser beam injects sample Pond, scattering light is received using photodetector, light intensity auto-correlation function is calculated using digital correlator, then send correlation function Enter computer and carry out data inversion, inverting obtains particle size distribution curve map.
The grain graininess point that Fig. 6 goes out for the light intensity auto-correlation function log inversion under the scattering angle after comprehensive multiple angles Cloth curve map and real particle size distribution curve map.The figure is with actual particle size error as little as 2%, illustrating this hair Bright apparatus and method are more accurate, truly feasible.
In the method measured using apparatus of the present invention, pass through the light intensity auto-correlation for measuring multiple different scattering angles Function is attached in a data analysis, is avoided the incorrect property selected the scattering angle of a unknown sample, can be obtained Varigrained particle obtains more metrical informations, and then obtain more accurately in the scattering properties of different scattering angles Particle size distribution.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., all should be included Within protection scope of the present invention.

Claims (8)

1. a kind of multi-peak particle swarm particle diameter distribution detection means, it is characterised in that it includes micro-fluidic chip (7), miniflow pump (6), laser (1), the first focus lens group (2), the second focus lens group (13), disk adjustment frame (3), photodetector (8), digital correlator (9) and computer (10), wherein,
Micro-fluidic chip (7) is arranged in disk adjustment frame (3), is provided with the micro-fluidic chip (7) as sample cell Flat fluid channel, flat fluid channel connection miniflow pump (6), miniflow pump (6) are used for the sample of grain diameter to be measured Flat fluid channel is pumped to,
Photodetector (8) is arranged in disk adjustment frame or is arranged on disk adjustment frame periphery,
First focus lens group (2) is arranged on laser (1) outgoing light direction, for the emergent light of laser (1) to be carried out Collimation and focusing, it is incident in the sample cell of micro-fluidic chip (7), passes through from the laser facula of the first focus lens group (2) outgoing Particle in sample cell scatters,
Second focus lens group (13) is used to the scattering light being emitted from sample cell converging to photodetector (8), the photoelectricity Detector (8) is arranged on the outgoing light direction of the second focus lens group (13), for institute's angle measurement in recruiting unit's time The number of photons of light is scattered at degree, the digital correlator (9) is used for according to the light intensity at discrete light subnumber acquisition institute measuring angle certainly Correlation function, the computer (10) are used for the particle diameter that sample is obtained according to the inverting of light intensity auto-correlation function.
2. a kind of multi-peak particle swarm particle diameter distribution detection means as claimed in claim 1, it is characterised in that the disk is adjusted Whole frame (3) includes outer disc (4), inner disk (5) and disk rotary rotating shaft, wherein, outer disc (4), inner disk (5) are coaxially set To put, disk rotary rotating shaft is arranged at the common axle center of outer disc (4) and inner disk (5),
Outer disc (4) and disk rotary rotating shaft can rotate along common axle center, and inner disk (5) is fixed.
A kind of 3. multi-peak particle swarm particle diameter distribution detection means as claimed in claim 2, it is characterised in that photodetector (8) have it is multiple, micro-fluidic chip (7) is arranged on fixed inner disk (5) axle center and gone out, and multiple photodetectors (8) set Put in the edge of outer disc, so that the scattering light of multiple angles can be received.
A kind of 4. multi-peak particle swarm particle diameter distribution detection means as claimed in claim 3, it is characterised in that photodetector (8) there are three, fix photodetector respectively in the outer disc relevant position corresponding to three angle of scatterings, while measure one group Dynamic scattering light corresponding to angle of scattering,
Photodetector (8) output light electric current accesses the digital correlator of triple channel, during work, outer disc is rotated, that can obtain The dynamic scattering light of a variety of different angles.
A kind of 5. multi-peak particle swarm particle diameter distribution detection means as claimed in claim 2, it is characterised in that photodetector (8) there is one, a photodetector (8) is arranged on disk adjustment frame periphery and fixed, micro-fluidic chip (7) It is arranged in rotatable disk rotary rotating shaft, during work, rotating circular disc rotary shaft is to rotate micro-fluidic chip (7), so as to make Photodetector (8) obtains the scattering light of multiple angles.
A kind of 6. multi-peak particle swarm particle diameter distribution detection means as claimed in claim 2, it is characterised in that photodetector (8) there is one, a photodetector (8) is arranged at the maximum annulus of outer disc, and micro-fluidic chip (7) is arranged on interior It is at the axle center of disk and fixed, during work, outer disc is rotated, to adjust photodetector direction, so as to make photoelectricity Detector (8) obtains the dynamic scattering light of multiple angles.
7. a kind of multi-peak particle swarm particle diameter distribution detection means as described in one of claim 1-6, it is characterised in that described Photodetector is photomultiplier or photon counter.
A kind of 8. multi-peak particle swarm particle diameter distribution detection means as claimed in claim 7, it is characterised in that the photon meter Number device is single photon counter, small-signal can be identified and extracted, from the accuracy for improving Monitoring Data.
CN201710889301.8A 2017-09-27 2017-09-27 A kind of multi-peak particle swarm particle diameter distribution detection means Pending CN107782642A (en)

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Application publication date: 20180309