CN110296986B - Nanoparticle sensor based on-chip intensive waveguide and sensing method thereof - Google Patents

Nanoparticle sensor based on-chip intensive waveguide and sensing method thereof Download PDF

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CN110296986B
CN110296986B CN201810238271.9A CN201810238271A CN110296986B CN 110296986 B CN110296986 B CN 110296986B CN 201810238271 A CN201810238271 A CN 201810238271A CN 110296986 B CN110296986 B CN 110296986B
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waveguide
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nanoparticles
nano particles
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CN110296986A (en
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肖云峰
唐水晶
俞骁翀
龚旗煌
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Peking University
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    • G01MEASURING; TESTING
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00Measuring arrangements characterised by the use of optical techniques
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    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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    • GPHYSICS
    • G01MEASURING; TESTING
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    • G01V8/12Detecting, e.g. by using light barriers using one transmitter and one receiver
    • G01V8/16Detecting, e.g. by using light barriers using one transmitter and one receiver using optical fibres
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84Systems specially adapted for particular applications
    • G01N2021/8472Investigation of composite materials
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

The invention discloses a nanoparticle sensor based on-chip dense waveguides and a sensing method thereof. The method comprises the steps that a single waveguide is horizontally wound on the surface of a substrate in the maximum density under the condition that coupling is not generated to form an intensive waveguide, when nanoparticles attached to the surface of the intensive waveguide are located in the evanescent field range of a waveguide mode, probe light is scattered or absorbed by the nanoparticles, a step signal which is sharply reduced is generated by transmission power, the step signal encodes the size information of the nanoparticles, and a computer judges whether the nanoparticles exist or not by identifying the step signal and obtains the size information of the nanoparticles; the dense waveguide has large sensing area, and is two orders of magnitude higher than that of a straight waveguide; meanwhile, the capture efficiency is high, and the time response is fast; a sphere with a radius of 100nm of nanoparticles that can be detected; in addition the scattering signal of the waveguide mode of TM polarization is 30 times the TE polarization.

Description

Nanoparticle sensor based on-chip intensive waveguide and sensing method thereof
Technical Field
The invention relates to a nanoparticle sensing technology, in particular to a nanoparticle sensor based on-chip intensive waveguides and a sensing method thereof.
Background
At present, relevant fields such as homeland security, environmental monitoring, early diagnosis and the like urgently need a detection platform which can realize in-situ, rapidness, ultrasensitiveness and repeatability of nano-scale particles. Among the various sensors, optical evanescent field sensors have attracted more and more attention due to a number of unique advantages, such as high sensitivity, no need for labels and non-invasiveness, etc. In recent years, relevant research has focused on exploring new mechanisms to improve the sensitivity of sensors. For example, the use of singular points in the microcavity, or in combination with plasmon enhancement effects, increases the sensitivity of the sensor to detection at the single biomolecule and monoatomic level. The nano-fiber exploits the concept of photoelastic scattering in the dark field to reduce the detection limit even to the quantum noise level. Although the sensitivity of these sensors has exceeded the requirements of current applications, the following aspects severely hamper their practical application: 1. the micro-nano resonant cavity has a very small sensing area, so that a very long time is required for capturing and characterizing the nano particles. Although nanofiber coils and arrays can increase the detection area, the low axial uniformity of the nanofiber, the difficulty of integrating with microfluidics, and the associated nanofiber fixtures limit the practical applications of such sensors. 2. High power densities in microcavities and plasmonic resonators can have a photodisruptive effect on biological molecules. 3. The preparation process of optical sensors such as nano optical fibers, micro cavities and semi-continuous plasmon thin films is difficult to realize accurate control, so that the prepared sensors have inconsistent performance. Therefore, in view of the rapid development of timely diagnostic devices, there is an urgent need to develop a highly reproducible sensing platform to achieve rapid and ultrasensitive detection of nanoparticles.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an on-chip dense waveguide-based nanoparticle sensor and a sensing method thereof, and non-labeled single nanoparticles are detected by utilizing the elastic scattering principle in a waveguide evanescent field.
It is an object of the present invention to propose a nanoparticle sensor based on-chip dense waveguides.
The nanoparticle sensor based on the on-chip dense waveguide of the present invention includes: the device comprises a substrate, a single waveguide, a light source device, a first optical fiber waveguide coupler, a second optical fiber waveguide coupler, a photoelectric detector, a data acquisition card and a computer; wherein, the single waveguide is wound on the plane of the upper surface of the substrate at the maximum density under the condition of not generating coupling, and the curvature radius of the wound shape is more than 5 μm so as to reduce the loss of light, thereby forming a dense waveguide on the surface of the substrate; a first optical fiber waveguide coupler is arranged at one end of the single waveguide, and a second optical fiber waveguide coupler is arranged at the other end of the single waveguide; the photoelectric detector is connected to the data acquisition card; the data acquisition card is connected to the computer; the light source device emits detection light, the detection light enters the dense waveguide through the first optical fiber waveguide coupler, and after being transmitted through the dense waveguide, the transmission light is received by the photoelectric detector through the second optical fiber waveguide coupler; the photoelectric detector converts the optical signal into an electric signal, transmits the electric signal to the data acquisition card for analog-to-digital conversion, transmits the data to the computer for data mean filtering processing and extracts a sensing signal; when the nano particles attached to the surface of the dense waveguide are positioned in the evanescent field range of the waveguide mode of the dense waveguide, the probe light is scattered or absorbed by the nano particles, the transmission power generates a step signal which sharply drops, the step signal encodes the size information of the nano particles, and the computer judges whether the nano particles exist or not by identifying the step signal and obtains the size information of the nano particles.
The substrate and the waveguide are made of materials with small loss to the detection light, the waveguide is made of silicon, the substrate is made of silicon dioxide on the silicon, and the thickness of the silicon dioxide is larger than or equal to 1 mu m.
The width and height of the cross section of a single waveguide are all hundreds of nanometers.
The first and second fiber waveguide couplers are gratings, fiber prisms or fiber taper-waveguide up-down contact couplers.
The light source device comprises a laser and a function generator, wherein the laser emits laser, and probe light with stable light intensity and set shape and frequency is formed by the function generator.
Another object of the present invention is to provide a nanoparticle sensing method based on-chip dense waveguides.
The invention discloses a nanoparticle sensing method based on an on-chip dense waveguide, which comprises the following steps of:
1) the light source device emits detection light which enters the dense waveguide through the first optical fiber waveguide coupler; after the light is transmitted through the dense waveguide,
the transmission light is received by the photoelectric detector through the second optical fiber waveguide coupler;
2) the photoelectric detector converts the optical signal into an electric signal and transmits the electric signal to the data acquisition card for analog-to-digital conversion and acquisition; then will be
The data are transmitted to a computer for mean value filtering processing and sensing signals are extracted;
3) when the nanoparticles attached to the surface of the dense waveguide are located within the evanescent field of the waveguide mode of the dense waveguide,
the detection light is scattered or absorbed by the nano-particles, and the transmission power generates a sharply reduced step signal
Size information of the nanoparticles is encoded;
4) the computer identifies the step signal and judges whether the nano-particles exist or not through the step signal, and the size of the nano-particles is further obtained
And (5) small information.
Wherein, in the step 4), the computer comprises the following steps by identifying the step signal:
a) dividing data in a time interval of data acquisition into a plurality of processing units, wherein in order to ensure that an algorithm is not influenced by a slowly varying signal caused by the environment when extracting a signal and simultaneously can identify two step signals with a close time interval, the time interval of the processing unit is not too long, and the time area is 0.06 s-0.1 s;
b) calculating the difference between the average values of the (N-1) th processing unit and the (N +1) th processing unit before and after the calculation, wherein N is a natural number more than or equal to 10;
c) and identifying the step by comparing the obtained difference with the noise level of the signal in the interval of the (N-M) th processing unit and the (N + M) th processing unit, thereby obtaining a step signal, wherein M is a natural number less than or equal to N, and M is more than or equal to 10 and less than or equal to 100.
Each step signal represents the detection of a nanoparticle, and the presence or absence of the nanoparticle is determined from the identified step signal.
Further, obtaining the size information of the nanoparticles through the step signal comprises the following steps:
a) obtaining the scattering efficiency caused by the nano particles on the surface of the waveguide according to the step signal, wherein the scattering efficiency is equal to the detected light intensity reduction power corresponding to the step divided by the total power of the detected light;
b) then, according to the size of the scattering efficiency, the particle size range of the nano particles is found on calibration data obtained by finite element simulation, so that the size of the nano particles at the moment is obtained.
In step b), obtaining calibration data through finite element simulation, comprising the following steps:
i. firstly, geometrically modeling the materials of the dense waveguide, the nano particles and the substrate according to actual parameters, and defining the refractive index and the absorption coefficient of the materials at the same time;
meshing the established geometric model;
and iii, performing light field simulation, setting light field boundary conditions, and solving Maxwell equations and electromagnetic field differential equations to obtain the scattering efficiency of the nano particles with different sizes on the waveguide, so as to obtain the calibration data of the sizes of the nano particles. The invention has the advantages that:
the method comprises the steps that a single waveguide is horizontally wound on the surface of a substrate in the maximum density under the condition that coupling is not generated to form an intensive waveguide, when nanoparticles attached to the surface of the intensive waveguide are located in the evanescent field range of a waveguide mode, probe light is scattered or absorbed by the nanoparticles, a step signal which is sharply reduced is generated by transmission power, the step signal encodes the size information of the nanoparticles, and a computer judges whether the nanoparticles exist or not by identifying the step signal and obtains the size information of the nanoparticles; the dense waveguide has large sensing area, and is two orders of magnitude higher than that of a straight waveguide; meanwhile, the capture efficiency is high, and the time response is fast; a sphere with a radius of 100nm of nanoparticles that can be detected; in addition the scattering signal of the waveguide mode of TM polarization is 30 times the TE polarization.
Drawings
FIG. 1 is a schematic diagram of one embodiment of an on-chip dense waveguide-based nanoparticle sensor of the present invention;
FIG. 2 is an electron microscope image of a dense waveguide of one embodiment of an on-chip dense waveguide-based nanoparticle sensor of the present invention;
FIG. 3 is an intensity diagram of the transverse magnetic mode and transverse electric mode of the waveguide of one embodiment of the on-chip dense waveguide-based nanoparticle sensor of the present invention, wherein (a) is the intensity diagram of the transverse magnetic TM mode of the waveguide, and (b) is the intensity diagram of the transverse electric TE mode of the waveguide;
FIG. 4 is a schematic diagram of a step signal obtained by one embodiment of the on-chip dense waveguide-based nanoparticle sensing method of the present invention;
FIG. 5 is a graph comparing the nanoparticle trapping efficiency of a dense waveguide to a straight waveguide obtained by one embodiment of the on-chip dense waveguide-based nanoparticle sensor of the present invention;
FIG. 6 is a graph comparing response times obtained by one embodiment of the on-chip dense waveguide-based nanoparticle sensor of the present invention, wherein (a) is a graph of the response time of a dense waveguide and (b) is a graph of the response time of a straight waveguide;
fig. 7 is a graph of the step signal versus the size of the nanoparticle according to an embodiment of the present invention, wherein (a) a statistical distribution of the step signal caused by different sizes of nanoparticles on the dense waveguide is obtained for experimental measurement, and (b) the uncertainty of the dense waveguide for the size measurement of the nanoparticle is given.
Detailed Description
The invention will be further elucidated by means of specific embodiments in the following with reference to the drawing.
As shown in fig. 1, the nanoparticle sensor based on the on-chip dense waveguide of the present embodiment includes: the device comprises a substrate, a single waveguide, a light source device, first and second optical fiber waveguide couplers 3 and 4, a photoelectric detector 5, a data acquisition card 6 and a computer; wherein, the light source device comprises a laser 1 and a function generator 2; the single waveguide is horizontally wound on the surface of the substrate at the maximum density under the condition that the curvature radius of the wound shape is more than 5 μm so as to reduce the loss of light, thereby forming a dense waveguide 7 on the surface of the substrate; a first fiber waveguide coupler 3 is arranged at one end of the single waveguide, and a second fiber waveguide coupler 4 is arranged at the other end of the single waveguide; the photoelectric detector 5 is connected to the data acquisition card 6; the data acquisition card 6 is connected to a computer.
In this embodiment, a single waveguide is horizontally wound on the surface of the substrate in a spiral shape, and an electron microscope image is shown in fig. 2; the width of the cross section of the single waveguide is 500nm, and the height of the cross section of the single waveguide is 220 nm; the substrate employs silicon dioxide formed on silicon.
Treating standard polystyrene small ball solution with ultrasonic atomizer to produce single nanometer particle, and depositing it in dense mediumOn the waveguide, the corresponding flow rate is set to 10mL min-1. A low noise photodetector and a data acquisition card are used to monitor the real time transmission power of the waveguide, the sampling rate of the data acquisition card is 100 kS/s.
As shown in fig. 3, the scattered signal of the waveguide mode of TM polarization is 30 times the TE polarization.
As shown in fig. 4, the standard polystyrene pellet with a radius of 100nm passes through the waveguide during the deposition process to detect the response curve of the light intensity transmittance of the light. Each step signal on fig. 4 represents that the waveguide detected a nanoparticle.
As shown in fig. 5, when the deposition range of the nanoparticles is in the order of hundreds of micrometers, the dense waveguide improves the capture efficiency of the nanoparticles by two orders of magnitude compared to the straight waveguide.
As shown in fig. 6, the dense waveguide has a response time 5 times or more that of the straight waveguide when the deposition area of the nanoparticles is 30 μm under the same test conditions.
As shown in fig. 7(a), when the dense waveguide detects standard polystyrene beads with different radii, the step signal detected by the dense waveguide increases as the size of the beads increases. In addition, because the evanescent potential field of the waveguide mode is not uniform at the waveguide surface, as shown in fig. 3, the sizes of the step signals (scattering efficiencies) caused when the same size of nanoparticles fall at different positions of the cross section of the dense waveguide are not the same. Fig. 7(b) shows the relation between the scattering efficiency of the nanoparticles on the waveguide and the radius of the nanoparticles and the position of the nanoparticles on the cross section of the dense waveguide. For TM mode probe light, the dense waveguide has a size uncertainty of about 10% when measuring polystyrene spheres. That is, when the dense waveguide detects a step signal with a scattering efficiency of 1%, the radius of the corresponding nanoparticle is 157.3 ± 14.6 nm.
Finally, it is noted that the disclosed embodiments are intended to aid in further understanding of the invention, but those skilled in the art will appreciate that: various substitutions and modifications are possible without departing from the spirit and scope of the invention and the appended claims. Therefore, the invention should not be limited to the embodiments disclosed, but the scope of the invention is defined by the appended claims.

Claims (4)

1. A nanoparticle sensing method based on-chip dense waveguides is characterized by comprising the following steps:
1) the light source device emits detection light which enters the dense waveguide through the first optical fiber waveguide coupler; after the transmission of the dense waveguide, the transmission light is received by the photoelectric detector through the second optical fiber waveguide coupler;
2) the photoelectric detector converts the optical signal into an electric signal and transmits the electric signal to the data acquisition card for analog-to-digital conversion and acquisition; then transmitting the data to a computer for mean value filtering processing and extracting a sensing signal;
3) when the nano particles attached to the surface of the dense waveguide are positioned in the evanescent field range of the waveguide mode of the dense waveguide, the probe light is scattered or absorbed by the nano particles, and the transmission power generates a step signal which sharply drops, wherein the step signal encodes the size information of the nano particles;
4) the computer identifies the step signal, and judges whether the nano-particles exist or not through the step signal, so as to further obtain the size information of the nano-particles:
a) dividing data in a time interval of data acquisition into a plurality of processing units, wherein in order to enable an algorithm to be free from the influence of a slowly varying signal caused by the environment when extracting a signal and simultaneously identify two step signals with a close time interval, the time area of the processing unit is 0.06 s-0.1 s;
b) calculating the difference between the average values of the (N-1) th processing unit and the (N +1) th processing unit before and after the calculation, wherein N is a natural number more than or equal to 10;
c) and identifying the step by comparing the obtained difference with the noise level of the signal in the interval of the (N-M) th processing unit and the (N + M) th processing unit, thereby obtaining a step signal, wherein M is a natural number less than or equal to N, and M is more than or equal to 10 and less than or equal to 100.
2. The sensing method of claim 1, wherein each step signal represents the detection of a nanoparticle, such that the presence or absence of a nanoparticle is determined from the identified step signals.
3. The sensing method of claim 1, wherein obtaining information on the size of the nanoparticle from the step signal comprises:
a) obtaining the scattering efficiency caused by the nano particles on the surface of the waveguide according to the step signal, wherein the scattering efficiency is equal to the detected light intensity reduction power corresponding to the step divided by the total power of the detected light;
b) then, according to the size of the scattering efficiency, the particle size range of the nano particles is found on calibration data obtained by finite element simulation, so that the size of the nano particles at the moment is obtained.
4. A sensing method according to claim 3, wherein in step b) calibration data is obtained by finite element simulation, comprising the steps of:
i. firstly, geometrically modeling the materials of the dense waveguide, the nano particles and the substrate according to actual parameters, and defining the refractive index and the absorption coefficient of the materials at the same time;
meshing the established geometric model;
and iii, performing light field simulation, setting light field boundary conditions, and solving Maxwell equations and electromagnetic field differential equations to obtain the scattering efficiency of the nano particles with different sizes on the waveguide, so as to obtain the calibration data of the sizes of the nano particles.
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