CN103018167A - Surface plasma resonance sample stage and preparation method thereof - Google Patents

Surface plasma resonance sample stage and preparation method thereof Download PDF

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Publication number
CN103018167A
CN103018167A CN2011102854845A CN201110285484A CN103018167A CN 103018167 A CN103018167 A CN 103018167A CN 2011102854845 A CN2011102854845 A CN 2011102854845A CN 201110285484 A CN201110285484 A CN 201110285484A CN 103018167 A CN103018167 A CN 103018167A
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Prior art keywords
surface plasma
sample stage
periodic array
metal nanoparticle
nanometers
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CN2011102854845A
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史丽娜
李海亮
杜宇禅
朱效立
李冬梅
谢常青
刘明
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Institute of Microelectronics of CAS
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Institute of Microelectronics of CAS
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Priority to CN2011102854845A priority Critical patent/CN103018167A/en
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Abstract

The invention discloses a surface plasma resonance sample stage and a preparation method thereof. The surface plasma resonance sample stage comprises a support structure, a metal film formed on the support structure, and a metal nanoparticle periodic array formed on the metal film and used for carrying a biological sample to be tested, wherein the Bragg scattering of the metal nanoparticle aperiodic array provides wave vector match needed by stimulation of the surface plasma of the biological sample to be tested. The surface plasma resonance sample stage utilizes the metal nanoparticle periodic array structure to stimulate the surface plasma, has a small volume and can be carried easily.

Description

Surface plasma body resonant vibration sample stage and preparation method thereof
Technical field
The present invention relates to the electron trade field of measuring technique, relate in particular to a kind of surface plasma body resonant vibration sample stage and preparation method thereof.
Background technology
Surface plasma is a kind of electromagnetic wave of propagating at metal and medium interface, is produced by incident field and metal surface electron interaction.The resonant condition of surface plasma is very responsive to metal surface 100 nanometers refractive index subtle change of medium in 300 nanometers.The surface plasma body resonant vibration sample stage is the main tool of characterising biological interaction of molecules.The ultimate principle of surface plasma body resonant vibration sample stage is the variation by recording surface plasma resonance angle or resonant wavelength, realizes the detection to metal surface test analyte refractive index.Compare with the sample stage of other type, sample stage based on surface plasma body resonant vibration comes recognition sample by the change that detects the sample refractive index, do not need fluorescence labels or other labels, can carry out original position, harmless and unmarked detection to biological sample, so the surface plasma body resonant vibration sample stage is free of contamination high sensitivity sample stage.
Typical surface plasma body resonant vibration sample stage generally adopts the Kretschmann prism structure, and the p polarized light incides the interface of prism and metallic film at a certain angle through prism.For certain incident angle and optical wavelength, prism provides the coupling of the wave vector between incident electromagnetic wave and the surface plasma.Yet, adopt the surface plasma body resonant vibration sample stage of Kretschmann prism structure bulky, not easy of integration and carry.
Summary of the invention
The technical matters that (one) will solve
For solving above-mentioned one or more technical matterss, the invention provides a kind of surface plasma body resonant vibration sample stage and preparation method thereof, to overcome the bulky shortcoming of sample stage.
(2) technical scheme
According to an aspect of the present invention, provide a kind of surface plasma body resonant vibration sample stage.This sample stage comprises: supporting construction; Be formed at the metallic film on the supporting construction; Be formed at the metal nanoparticle periodic array on the metallic film, be used for carrying biological sample to be measured, provided by the Bragg diffraction of metal nanoparticle periodic array to excite the needed wave vector coupling of biological sample surface plasma to be measured.
Preferably, in the surface plasma body resonant vibration sample stage of the present invention, the metal nanoparticle periodic array is square lattice to be arranged, and the cycle is between 600 nanometer to 800 nanometers.
Preferably, in the surface plasma body resonant vibration sample stage of the present invention, for the single metal nano particle in the metal nanoparticle periodic array, its height is between 25 nanometer to 75 nanometers; It is shaped as disc or rectangle; When it was shaped as disc, disk diameter was between 300 nanometer to 600 nanometers; When it was shaped as rectangle, the rectangle length of side was between 300 nanometer to 600 nanometers.
Preferably, in the surface plasma body resonant vibration sample stage of the present invention, the material of metallic film and metal nanoparticle periodic array is gold, silver or aluminium.
Preferably, in the surface plasma body resonant vibration sample stage of the present invention, supporting construction is self-supporting film, silicon substrate, fused quartz substrate, simple glass substrate or organic glass substrate.
A kind of method of preparation table surface plasma resonance sample stage also is provided according to another aspect of the present invention.The method comprises: form metallic film in supporting construction; Form the metal nanoparticle periodic array at metallic film, carrying biological sample to be measured, provide excitating surface plasma needed wave vector coupling by the Bragg diffraction of metal nanoparticle periodic array.
(3) beneficial effect
Surface plasma body resonant vibration sample stage of the present invention and preparation method thereof has following beneficial effect:
(1) surface plasma body resonant vibration sample stage of the present invention adopts metal nanoparticle periodic structure excitating surface plasma, and volume is little, is easy to carry about with one;
(2) preparation method of surface plasma body resonant vibration sample stage of the present invention is lower to the processing technology requirement, and is compatible with traditional semiconductor technology, is easy to integrated.
(3) in the surface plasma body resonant vibration sample stage of the present invention, the Reflective Spectrum Characteristics of different cycles structure is different, and the researchist can make the nanostructured of different cycles size as required, satisfies the measurement in the different wave length situation.
Description of drawings
Fig. 1 is the sectional view of embodiment of the invention surface plasma body resonant vibration sample stage;
Fig. 2 is the vertical view of embodiment of the invention surface plasma body resonant vibration sample stage metal nanoparticle periodic array;
Fig. 3 is the synoptic diagram that embodiment of the invention surface plasma body resonant vibration sample stage is tested;
Fig. 4 is the reflection spectrogram that embodiment of the invention surface plasma body resonant vibration sample stage is tested the biological material specimens of different refractivity;
Fig. 5 is the Reflective Spectrum Characteristics figure of the surface plasma body resonant vibration sample stage of the different gold dish of the present invention diameter;
Fig. 6 is the Reflective Spectrum Characteristics figure of the surface plasma body resonant vibration sample stage of different cycles structure of the present invention;
Fig. 7 is the process flow diagram of embodiment of the invention preparation table surface plasma resonance sample stage method.
Embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
In one exemplary embodiment of the present invention, a kind of surface plasma body resonant vibration sample stage based on the metal nanoparticle periodic array is disclosed.Fig. 1 is the sectional view of embodiment of the invention surface plasma body resonant vibration sample stage.As shown in Figure 1, this surface plasma body resonant vibration sample stage comprises what supporting construction (white portion) 1, metallic film 2 and metal nanoparticle periodic array 3 (left diagonal line hatches zone) formed.Series of liquid biological samples to be measured is coated on the metal nanoparticle periodic array.
In the present embodiment, the material of metallic film and metal nanoparticle is identical or different.Preferably, the material of metallic film and metal nanoparticle periodic array is all gold, silver or aluminium.And supporting construction can be self-supporting film (comprising Kapton, carborundum films or silicon nitride film), fused quartz, simple glass, organic glass or silicon.
Fig. 2 is the vertical view of embodiment of the invention surface plasma body resonant vibration sample stage metal nanoparticle periodic array.As shown in Figure 2, the metal nanoparticle periodic array is square lattice to be arranged, and the cycle is between 600 nanometers, 800 nanometers.For the single metal nano particle in the metal nanoparticle periodic array, its height is between 25 nanometer to 75 nanometers; It is shaped as disk or rectangular parallelepiped; When it was shaped as disk, diameter was between 300 nanometer to 600 nanometers; When it was shaped as rectangular parallelepiped, the length of side was between 300 nanometer to 600 nanometers.Need to prove, although the metal nanoparticle periodic array is the square lattice periodic arrangement in the present embodiment, but its arrangement mode is not limited to this, for example, the metal nanoparticle periodic array also can be the pane subcycle and arrange, for rectangular grid, they can be between 600 nanometers between 800 nanometers in cycle of one dimension, can be between 600 nanometers between 800 nanometers in the cycle of another dimension.
Fig. 3 is the synoptic diagram that embodiment of the invention surface plasma body resonant vibration sample stage is tested.As shown in Figure 3, the detection light that is sent by light source 5 impinges perpendicularly on the light tight metallic film 2 through behind the part reflective semitransparent film 7; Be distributed with a plurality of metal nanoparticles on the light tight metallic film 2; Metal nanoparticle is period profile, surveying light impinges perpendicularly on the metal nanoparticle array, Bragg diffraction by array provides excitating surface plasma required wave vector coupling, at this moment can produce surface plasma resonance at some wavelength, surface plasma resonance pattern and testing liquid interact, then reflected light is along the vertical outgoing of input path, and through part reflective semitransparent film 7, last reflected light is received by photo-detector 6.
Below the principle and feature of surface plasma body resonant vibration sample stage of the present invention is described.For simplicity, below in the explanation, the material of metallic film and metal nanoparticle is gold, and the shape of gold nano grain is disc, abbreviation gold dish; Gold thin film is called for short golden film.
Fig. 4 is the reflection spectrogram that embodiment of the invention surface plasma body resonant vibration sample stage is tested the biological material specimens of different refractivity.Golden film thickness 55 nanometers in the used surface plasma resonance sensor structure, gold nano structural thickness 50 nanometers, gold dish diameter 465 nanometers, the gold dish is square lattice periodic arrangement, cycles 700 nanometer.As shown in Figure 4, when metal surface test analyte refractive index changed to 1.33 from 1.30, surface plasma wave length was from 707.03 nanometer red shifts to 717.86 nanometers.The sensitivity that can get thus surface plasma resonance sensor is:
S ( λ , n 1 , n 2 ) = lim Δn → 0 λ ( n 1 ) - λ ( n 2 ) n 1 - n 2 = 717.86 - 707.03 1.33 - 1.30 = 361 nm / RIU .
Fig. 5 is the Reflective Spectrum Characteristics figure of the surface plasma body resonant vibration sample stage of the different gold dish of the present invention diameter.Golden film thickness 55 nanometers in the used surface plasma resonance sensor, gold nano structural thickness 50 nanometers, gold dish diameter is respectively 310,465 and 620 nanometers, and the gold dish is the square lattice periodic arrangement, and the cycle is 700 nanometers, determinand refractive index 1.30.As shown in Figure 5, increase with disk diameter, the surface plasma body resonant vibration wavelength is followed successively by 716.72,717.86 and 716.72 nanometers, the essentially no variation in the position of resonant wavelength, the impact of the big or small effects on surface plasma resonance wavelength of this explanation metal nanoparticle is less, therefore this surface plasma resonance sensor structure is lower to the processing technology requirement, and is compatible with traditional semiconductor technology.
Fig. 6 is the Reflective Spectrum Characteristics figure of the surface plasma body resonant vibration sample stage of different cycles structure of the present invention.Metallic film is golden film in the used surface plasma resonance sensor structure, its thickness 55 nanometers; Thickness 50 nanometers of gold nano grain are disc, and its diameter is 465 nanometers.Gold nano grain is the square lattice periodic arrangement, and the periodic structure of three samples is respectively 600,650 and 700 nanometers, and biological sample refractive index to be measured is 1.30.As can be seen from Figure 4, increase the surface plasma body resonant vibration red shift of wavelength with the cycle.This specific character of metal nanoparticle periodic array makes the researchist can make as required the nanostructured of different cycles size, satisfies the measurement in the different wave length situation.
A kind of method of preparation table surface plasma resonance sample stage also is provided according to another aspect of the present invention.Fig. 7 is the process flow diagram of embodiment of the invention preparation table surface plasma resonance sample stage method.As shown in Figure 7, the method may further comprise the steps:
Step S702, the golden film of electron beam evaporation 55 nanometers on silicon substrate;
Step S704, spin coating electron sensitive resist ZEP520A on golden film, front baking is removed the solvent in the resist;
Step S706 carries out electron beam exposure according to the periodic array domain of making in advance to electron sensitive resist, and then the special-purpose developer solution N50 with ZEP520A develops, and uses the isopropyl alcohol photographic fixing again, to remove the electron sensitive resist of predetermined period array position;
Step S708, at the metallic film gold coated films that powers on, the thickness of gold thin film is 50 nanometers, need to prove, for simplicity, has adopted the mode of electroplating, and also can adopt the methods such as thermal evaporation, sputter;
Step S710 removes electron sensitive resist ZEP520A with the special use of the ZEP520A liquid ZMDAC that removes photoresist, and the electron sensitive resist ZEP520A outside periodic array is removed thereupon, and sample stage is finished making.
In sum, surface plasma body resonant vibration sample stage of the present invention and preparation method thereof has following beneficial effect:
(1) surface plasma body resonant vibration sample stage of the present invention adopts metal nanoparticle periodic structure excitating surface plasma, and volume is little, is easy to carry about with one;
(2) preparation method of surface plasma body resonant vibration sample stage of the present invention is lower to the processing technology requirement, and is compatible with traditional semiconductor technology, is easy to integrated.
(3) in the surface plasma body resonant vibration sample stage of the present invention, the Reflective Spectrum Characteristics of different cycles structure is different, and the researchist can make the nanostructured of different cycles size as required, satisfies the measurement in the different wave length situation.
Above-described specific embodiment; purpose of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the above only is specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (10)

1. a surface plasma body resonant vibration sample stage is characterized in that, comprising:
Supporting construction;
Be formed at the metallic film on the described supporting construction;
Be formed at the metal nanoparticle periodic array on the described metallic film, be used for carrying biological sample to be measured, provided by the Bragg diffraction of described metal nanoparticle periodic array to excite the needed wave vector coupling of described biological sample surface plasma to be measured.
2. surface plasma body resonant vibration sample stage according to claim 1 is characterized in that, described metal nanoparticle periodic array is square lattice to be arranged, and the cycle is between 600 nanometer to 800 nanometers.
3. surface plasma body resonant vibration sample stage according to claim 1 is characterized in that, for the single metal nano particle in the described metal nanoparticle periodic array,
Its height is between 25 nanometer to 75 nanometers;
It is shaped as disc or rectangle;
When it was shaped as disc, disk diameter was between 300 nanometer to 600 nanometers; When it was shaped as rectangle, the rectangle length of side was between 300 nanometer to 600 nanometers.
4. surface plasma body resonant vibration sample stage according to claim 1, the material of described metallic film and described metal nanoparticle periodic array is gold, silver or aluminium.
5. each described surface plasma body resonant vibration sample stage in 4 according to claim 1 is characterized in that described supporting construction is self-supporting film, silicon substrate, fused quartz substrate, simple glass substrate or organic glass substrate.
6. the method for a preparation table surface plasma resonance sample stage is characterized in that, comprising:
Form metallic film in supporting construction;
Form the metal nanoparticle periodic array at described metallic film, carrying biological sample to be measured, provide excitating surface plasma needed wave vector coupling by the Bragg diffraction of described metal nanoparticle periodic array.
7. the method for preparation table surface plasma resonance sample stage according to claim 6 is characterized in that, described metal nanoparticle periodic array is square lattice to be arranged, and the cycle is between 600 nanometers, 800 nanometers.
8. the method for preparation table surface plasma resonance sample stage according to claim 6 is characterized in that, for the single metal nano particle in the described metal nanoparticle periodic array,
Its height is between 25 nanometer to 75 nanometers;
It is shaped as disc or rectangle;
When it was shaped as disc, disk diameter was between 300 nanometer to 600 nanometers; When it was shaped as rectangle, the rectangle length of side was between 300 nanometer to 600 nanometers.
9. the method for preparation table surface plasma resonance sample stage according to claim 6, the material of described metallic film and described metal nanoparticle periodic array is gold, silver or aluminium.
10. the method for each described preparation table surface plasma resonance sample stage in 9 according to claim 6 is characterized in that, the described step that forms the metal nanoparticle periodic array at metallic film comprises:
Spin coating electron sensitive resist on described metallic film;
According to default periodic array template described electron sensitive resist is carried out photoetching and development, to remove the electron sensitive resist of predetermined period array position;
Plated metal on the metallic film of described predetermined period array position;
Remove electron sensitive resist, the metal outside described periodic array position is removed thereupon.
CN2011102854845A 2011-09-23 2011-09-23 Surface plasma resonance sample stage and preparation method thereof Pending CN103018167A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105259141A (en) * 2015-10-30 2016-01-20 山东大学 Surface plasma resonance high-refractive-index sensor based on porous aluminum membrane structure and application thereof
CN106356311A (en) * 2015-07-16 2017-01-25 格罗方德半导体公司 Inline buried metal void detection by surface plasmon resonance (spr)
CN113474637A (en) * 2018-11-29 2021-10-01 乐卓博大学 Method for identifying structures

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Publication number Priority date Publication date Assignee Title
CN1468385A (en) * 2000-07-21 2004-01-14 �Ƹ��� Surface plasmon polariton band gap structures
US20060072114A1 (en) * 2004-10-06 2006-04-06 Sigalas Mihail M Apparatus and mehod for sensing with metal optical filters
US20060279738A1 (en) * 2005-06-08 2006-12-14 Canon Kabushiki Kaisha Sensing element used in sensing device for sensing target substance in specimen by using plasmon resonance
CN101339128A (en) * 2008-08-27 2009-01-07 中国科学院光电技术研究所 Surface plasma resonance image-forming nanostructure array chip preparation method
CN101933116A (en) * 2008-02-05 2010-12-29 尼尔技术有限责任公司 A method for performing electron beam lithography

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1468385A (en) * 2000-07-21 2004-01-14 �Ƹ��� Surface plasmon polariton band gap structures
US20060072114A1 (en) * 2004-10-06 2006-04-06 Sigalas Mihail M Apparatus and mehod for sensing with metal optical filters
US20060279738A1 (en) * 2005-06-08 2006-12-14 Canon Kabushiki Kaisha Sensing element used in sensing device for sensing target substance in specimen by using plasmon resonance
CN101933116A (en) * 2008-02-05 2010-12-29 尼尔技术有限责任公司 A method for performing electron beam lithography
CN101339128A (en) * 2008-08-27 2009-01-07 中国科学院光电技术研究所 Surface plasma resonance image-forming nanostructure array chip preparation method

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106356311A (en) * 2015-07-16 2017-01-25 格罗方德半导体公司 Inline buried metal void detection by surface plasmon resonance (spr)
CN106356311B (en) * 2015-07-16 2019-04-02 格罗方德半导体公司 It is detected by the consistent embedment metal cavity of surface plasma body resonant vibration (SPR)
CN105259141A (en) * 2015-10-30 2016-01-20 山东大学 Surface plasma resonance high-refractive-index sensor based on porous aluminum membrane structure and application thereof
CN105259141B (en) * 2015-10-30 2018-08-03 山东大学苏州研究院 It is a kind of based on the surface plasma resonance high refractive index sensor of porous aluminium structure and its application
CN113474637A (en) * 2018-11-29 2021-10-01 乐卓博大学 Method for identifying structures

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Application publication date: 20130403