CN104792746B - A kind of detection method being imaged using surface phasmon scattering to nano-substance - Google Patents

A kind of detection method being imaged using surface phasmon scattering to nano-substance Download PDF

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CN104792746B
CN104792746B CN201410751328.7A CN201410751328A CN104792746B CN 104792746 B CN104792746 B CN 104792746B CN 201410751328 A CN201410751328 A CN 201410751328A CN 104792746 B CN104792746 B CN 104792746B
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nano
substance
light
detection method
surface phasmon
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CN104792746A (en
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路鑫超
刘虹遥
陈鲁
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Institute of Microelectronics of CAS
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Institute of Microelectronics of CAS
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Abstract

The present invention discloses a kind of detection method being imaged using surface phasmon scattering to nano-substance, and the detection method includes:Gold coated films on the cover slip;Adhere to nano-substance in the gold thin film;The light that light source is sent out focuses on the back focal plane of oil immersion objective with p-polarization state after expanding shaping;Position of the incident light on the back focal plane of oil immersion objective is adjusted, makes incident light is oblique to be mapped on the coverslip, in the gold thin film surface excitation surface phasmon, the surface phasmon is propagated along gold thin film surface, and scattering is generated with the nano-substance;Generated surface phasmon scattering is converted into optical signal and is collected together with reflected light by oil immersion objective;The collected reflected light for including surface phasmon scattered signal is imaged by CCD.

Description

A kind of detection method being imaged using surface phasmon scattering to nano-substance
Technical field
The present invention relates to nano-substance detection technique fields more particularly to a kind of utilization surface phasmon to scatter to nanometer The detection method that substance is imaged.
Background technology
In recent years, with the continuous development of nanometer science and technology, people are more and more to the concern of nano-substance, such as Carbon nanotube, quantum dot and virus etc..Since microscopical resolution ratio is by using wavelength to be limited, optical diffraction limit So that light microscope can not substance of the detected size less than 200 nanometers.
And electron wavelength is far smaller than optical wavelength, and therefore, nano-substance can be imaged using electron microscope Detection.Electron microscope mainly includes transmission electron microscope (TEM) and scanning electron microscope (SEM), is made using electron beam For light source, diffraction limit can be broken through, microscopical resolution ratio is increased to nanometer scale.But due to electron beam penetration power Weak, the sample detected using transmission electron microscope is necessary for ultra-thin section, therefore, higher to sample requirement.And scan electricity Sub- microscope then needs sample conductive, and sweep time is long.And both electron microscopes are required to vacuumizing, Make entire instrument cost high, it is bulky, it is difficult to mobile.
In addition, scanning tunneling microscope (STM) generates electron tunneling effect using probe and sample surfaces, tunnel electricity is utilized Stream obtains sample surface information, has the high-resolution of atom magnitude, but this microscope also requires sample conductive. Atomic force microscope (AFM) can be used for detecting insulator sample, using needle point and the slight active force of sample surfaces, to sample Surface is detected, and this microscope sweep time is long, it is also desirable to vacuumizing, it is of high cost.
Therefore, the above-mentioned microscopy available for nano-substance detection is stringent to sample requirement, and sweep time is long, can not Testing result is quickly obtained, needs vacuumizing, it is of high cost, volume is big.
Invention content
The application provides a kind of detection method being imaged using surface phasmon scattering to nano-substance, solves Detection method of the prior art is stringent to sample requirement, and sweep time is long, can not be quickly obtained testing result, vacuum is needed to grasp Make, of high cost, bulky technical problem.
The application provides a kind of detection method being imaged using surface phasmon scattering to nano-substance, the inspection Survey method includes:Gold coated films on the cover slip;Adhere to nano-substance in the gold thin film;The light that light source is sent out is by expanding After shaping, the back focal plane of oil immersion objective is focused on p-polarization state;Adjust position of the incident light on the back focal plane of oil immersion objective Put, make incident light is oblique to be mapped on the coverslip, the gold thin film surface excitation surface phasmon, described surface etc. from Excimer is propagated along gold thin film surface, and scattering is generated with the nano-substance;The surface phasmon scattering is converted into optical signal It is collected with together with reflected light by oil immersion objective;Collected light is imaged by CCD.
Preferably, it is described that collected light is imaged by CCD, including:It is measured with CCD without any nano-substance Reflected light is as background hot spot;There is the reflected light of the nano-substance as current hot spot by the use of CCD measurements;By the background hot spot Subtract each other with the current hot spot, obtain the nano-substance and cause surface phasmon scattered field.
Preferably, the nano-substance is one or more in virus, nano particle, carbon nanotube, quantum dot.
Preferably, the light source is laser or Light-Emitting Diode, and the wave-length coverage of the light is received for 355 nanometers~800 Rice.
Preferably, the surface phasmon is excited using Kretschmann (gram Lay Schumann) structure.
Preferably, the thickness range of the gold thin film is 30 nanometers~60 nanometers.
Preferably, range NA=1.0~1.7 of the oil immersion objective.
Preferably, the oblique incidence angle being mapped on the coverslip of the incident light is 30 degree of -60 degree.
Preferably, the gold thin film surface can be air or liquid medium.
The application has the beneficial effect that:
Above-mentioned detection method utilizes object lens coupled modes excitating surface phasmon, and the light sent out by light source is by expanding After shaping, the back focal plane of oil immersion objective is focused on p-polarization state, adjusts position of the incident light on the back focal plane of oil immersion objective It puts, makes incident light is oblique to be mapped on the coverslip, the evanescent wave wave vector for the total reflection that high refractive index coverslip generates and surface Phasmon wave vector matches, and in the gold thin film surface excitation surface phasmon, the surface phasmon is along gold thin film Surface is propagated, and generates scattering with the nano-substance, generated surface phasmon scattering is converted into optical signal and reflected light It is collected together by the oil immersion objective;Collected light is imaged by CCD again, you can obtain inspection result, solve Detection method of the prior art is stringent to sample requirement, and sweep time is long, can not be quickly obtained testing result, vacuum is needed to grasp Make, of high cost, bulky technical problem.
Description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, embodiment will be described below Needed in attached drawing be briefly described, it should be apparent that, the accompanying drawings in the following description be only the present invention some Embodiment.
Fig. 1 is the detection that one better embodiment of the application is imaged nano-substance using surface phasmon scattering The flow chart of method;
Fig. 2 is the structure diagram of detection device that the detection method in Fig. 1 uses;
Fig. 3 is to 1 micron of nano-substance image using the detection method in Fig. 1;
Fig. 4 is to 500 nanometers of nano-substance image using the detection method in Fig. 1;
Fig. 5 is to 200 nanometers of nano-substance image using the detection method in Fig. 1;
Fig. 6 is to 100 nanometers of nano-substance image using the detection method in Fig. 1;
Fig. 7 is to 57.7 nanometers of nano-substance image using the detection method in Fig. 1;
Fig. 8 is to 39 nanometers of nano-substance image using the detection method in Fig. 1;
Fig. 9 is using the scattered power of the detection method in Fig. 1 and particle size relational graph.
Specific embodiment
In order to better understand the above technical scheme, in conjunction with appended figures and specific embodiments to upper Technical solution is stated to be described in detail.
Fig. 1 is the detection that one better embodiment of the application is imaged nano-substance using surface phasmon scattering The flow chart of method.The detection method is performed by detection device shown in Fig. 2.The detection device includes light source 210, line Polarizer 220, pellicular beamsplitters 230, oil immersion objective 240, coverslip 250 and CCD260.CCD full name are Charge-coupled Device, charge coupled cell.It is described that detection method includes the following steps.
Step 110, the gold coated films on coverslip 250.In the present embodiment, the thickness of the metallic film is received for 50 Rice, in other embodiments, the thickness of the metallic film can carry out as needed.
Step 120, adhere to nano-substance in the gold thin film.The nano-substance is nano-substance to be detected.Institute Stating nano-substance, to be specifically as follows virus, nano particle, carbon nanotube, quantum dot etc. therein one or more.
Step 130, the light that light source 210 is sent out is after expanding shaping, after focusing on oil immersion objective 240 with p-polarization state Focal plane.That is, this method, using Kretschmann structures, the mode coupled using oil immersion objective uses oil immersion As wave vector compensatory device.The light source 210 is specially laser or Light-Emitting Diode.The advantages of mode of oil immersion objective coupling It is:Incident light can be made parallel with reflected light, by changing position of the incident light on oil immersion objective back focal plane, adjust and swash The incidence angle of surface phasmon is sent out, angular adjustment is converted into easy one-dimensional length adjustment, makes apparatus structure compact, steady It is fixed.
Specifically, after the light that the light source 210 is sent out realizes p-polarization state via the linear polarizer 220, then by described thin Film beam splitter 230 reflects.The sequence of step 120 and step 130 can be swapped or is carried out at the same time.In present embodiment In, the wave-length coverage of the light is 355 nanometers~800 nanometers.In the present embodiment, the numerical aperture model of the oil immersion objective NA=1.0~1.7 are enclosed, and with directional light oblique incidence excitating surface phasmon, it is ensured that the big imaging more than 100 microns The visual field.
Step 140, position of the incident light on the back focal plane of oil immersion objective 240 is adjusted, makes incident light is oblique to be mapped to institute It states on coverslip 250, evanescent wave wave vector and the surface phasmon wave vector of the total reflection that high refractive index coverslip 250 generates Match, it is and described in the gold thin film surface excitation surface phasmon, the surface phasmon is propagated along gold thin film surface Nano-substance generates scattering.The oblique incidence angle being mapped on the coverslip of the incident light is adjusted, can be inspired most strong Surface phasmon corresponds to most weak reflected light, using CCD260 it is observed that surface phasmon most excites by force at this time.It is excellent Selection of land, the oblique ranges of incidence angles being mapped on the coverslip of the incident light are spent for 30 degree -60, and the gold thin film surface can be with For air or liquid medium.When air dielectric is in the surface of the gold thin film, incidence angle is 36.8 degree, is detected on CCD Object lens collect reflected light it is most weak;When liquid medium is in the surface of the gold thin film, incidence angle is 54 degree.
It after surface phasmon is excited on gold thin film surface, propagates along gold thin film surface, adheres on gold thin film surface During nano-substance, surface phasmon encounters nano-substance in communication process can generate scattering, and a part is dispersed into space Spatially angle is distributed, and another part is then radially scattered along the propagation generation of gold thin film surface, due to surface phasmon space scattering Loss is very big, so only considering the interface scattering that surface phasmon is propagated on gold thin film surface herein.Along gold thin film surface Interference effect is generated between the interface scattering of propagation and the surface phasmon remotivated, light and shade can be generated on gold thin film surface Alternate fringe distribution, and in concentric parabolic shape, and it is strong to generate near nano-substance surface phasmon local .
Step 150, the surface phasmon scattering is converted into optical signal and is received together with reflected light by the oil immersion objective Collection, is imaged collected light by CCD.As the inverse process of excited by visible light surface phasmon, surface etc. from sharp First interface scattering can be converted into optical signal in communication process, therefore, in reflected light contain surface phasmon scattering letter Number, collected light is imaged, and imaging data is handled using CCD, can realize and surface phasmon is scattering into Picture.
In order to reduce the background noise to the influence of signal, it is described by CCD to including surface phasmon scattered signal Reflected light be imaged, specifically include:The reflected light without any nano-substance is measured as background hot spot by the use of CCD;It is surveyed with CCD Amount has the reflected light of the nano-substance as current hot spot;The background hot spot and the current hot spot are subtracted each other, into line number According to average noise reduction process, the ambient noise of flare and the noise of CCD are removed, enhances the contrast of scattered field and background, obtains It obtains the nano-substance and causes surface phasmon scattered field.
The light that above-mentioned detection method is sent out by light source 210 focuses on oil immersion objective after expanding shaping, with p-polarization state 240 back focal plane adjusts position of the incident light on the back focal plane of oil immersion objective 240, make incident light it is oblique be mapped to it is described On coverslip 250, the evanescent wave wave vector for the total reflection that high refractive index coverslip 250 generates is matched with surface phasmon wave vector, With in the gold thin film surface excitation surface phasmon, the surface phasmon is propagated along gold thin film surface, is received with described Rice substance generates scattering, and generated surface phasmon scattering is converted into optical signal and is received together with reflected light by oil immersion objective Collection, then collected light is imaged by CCD, you can inspection result is obtained, solves detection method of the prior art Stringent to sample requirement, sweep time is long, can not be quickly obtained testing result, needs vacuumizing, of high cost, bulky skill Art problem.
Although preferred embodiments of the present invention have been described, but those skilled in the art once know basic creation Property concept, then additional changes and modifications may be made to these embodiments.So appended claims be intended to be construed to include it is excellent It selects embodiment and falls into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art God and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies Within, then the present invention is also intended to include these modifications and variations.

Claims (8)

  1. A kind of 1. detection method being imaged using surface phasmon scattering to nano-substance, which is characterized in that the inspection Survey method includes:
    Gold coated films on the cover slip;
    Adhere to nano-substance in the gold thin film;
    The light that light source is sent out focuses on the back focal plane of oil immersion objective with p-polarization state after expanding shaping;
    Position of the incident light on the back focal plane of oil immersion objective is adjusted, makes incident light is oblique to be mapped on the coverslip, in institute Gold thin film surface excitation surface phasmon is stated, the surface phasmon is propagated along gold thin film surface, with the nano-substance Generate scattering;
    The surface phasmon scattering is converted into optical signal and is collected together with reflected light by the oil immersion objective, passes through CCD pairs Collected light is imaged;
    Wherein, it is described that collected light is imaged by CCD, including:
    The reflected light without any nano-substance is measured as background hot spot by the use of CCD;
    There is the reflected light of the nano-substance as current hot spot by the use of CCD measurements;
    The background hot spot and the current hot spot are subtracted each other, the nano-substance is obtained and causes surface phasmon scattered field.
  2. 2. detection method as described in claim 1, which is characterized in that the nano-substance is virus, nano particle, carbon nanometer It is one or more in pipe, quantum dot.
  3. 3. detection method as described in claim 1, which is characterized in that the light source be laser or Light-Emitting Diode, it is described The wave-length coverage for the light that light source is sent out is 355 nanometers~800 nanometers.
  4. 4. detection method as described in claim 1, which is characterized in that excited using Kretschmann (gram Lay Schumann) structure The surface phasmon.
  5. 5. detection method as described in claim 1, which is characterized in that the thickness range of the gold thin film is received for 30 nanometers~60 Rice.
  6. 6. detection method as described in claim 1, which is characterized in that the range NA=1.0 of the oil immersion objective ~1.7.
  7. 7. detection method as described in claim 1, which is characterized in that the incident light is oblique to be mapped to entering on the coverslip Elevation range is 30 degree of -60 degree.
  8. 8. detection method as described in claim 1, which is characterized in that the gold thin film surface can be that air or liquid are situated between Matter.
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CN108051362B (en) * 2017-11-09 2021-10-08 中国科学院微电子研究所 Detection method for single nano-particle
CN109239020B (en) * 2018-09-17 2023-11-17 中国科学技术大学 Surface wave imaging system based on rotary illumination
CN110361364B (en) * 2019-07-29 2021-11-02 中国科学院微电子研究所 Micro-nano structure imaging method and device
CN112557352B (en) * 2019-09-26 2022-09-16 中国科学院微电子研究所 Excitation device of surface plasmon standing wave
CN112557262B (en) * 2019-09-26 2022-12-09 中国科学院微电子研究所 Detection method and detection device for single nano-particles
CN112525806B (en) * 2020-10-19 2023-04-25 中国科学院微电子研究所 Flow cell detection device, preparation method and system

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