CN103630515B - A kind of nano Au particle sensor and preparation method thereof - Google Patents
A kind of nano Au particle sensor and preparation method thereof Download PDFInfo
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- CN103630515B CN103630515B CN201310689966.6A CN201310689966A CN103630515B CN 103630515 B CN103630515 B CN 103630515B CN 201310689966 A CN201310689966 A CN 201310689966A CN 103630515 B CN103630515 B CN 103630515B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/55—Specular reflectivity
- G01N21/552—Attenuated total reflection
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- G01N21/84—Systems specially adapted for particular applications
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- G01N21/8507—Probe photometers, i.e. with optical measuring part dipped into fluid sample
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/85—Investigating moving fluids or granular solids
- G01N21/8507—Probe photometers, i.e. with optical measuring part dipped into fluid sample
- G01N2021/8528—Immerged light conductor
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Abstract
The present invention is to provide a kind of nano Au particle sensor and preparation method thereof.The end face of multi-core fiber is frustum structure, frustum surface is coated with total reflection film, the fiber end face being coated with total reflection film is fixed with the nano Au particle of rule arrangement, exciting light is injected in a fibre core of multi-core fiber, exciting light is reflected onto fiber end face place at frustum plated film place and in fiber end face experiences total internal reflection, the local surface plasma resonance effect of the evanscent field excitation nano gold particle produced, reflected light is by collecting, by the change of reflected light spectrum perception external substance physical quantity with the symmetrical moral fibre core of the fibre core injecting exciting light.Multi-core fiber, near-field optical tweezers self-assembling technique combine with nano Au particle local surface plasma resonance effect by the present invention, the near-field optical tweezers utilizing multi-core fiber to form can be caught nano Au particle, make nano Au particle carry out optics self assembly regular array according to the capture region regularity of distribution, structure is simple, volume is less, repeatability is high.
Description
Technical field
What the present invention relates to is a kind of Fibre Optical Sensor, the present invention also relates to a kind of preparation method of Fibre Optical Sensor.Specifically a kind of nano Au particle sensor and preparation method thereof.
Background technology
Nano Au particle refers to the molecule of diameter at the gold of 1 ~ 100nm, and General Decentralized is in the hydrosol.As far back as Middle Ages nano Au particle be just subject to people's attention because of the optical property of its uniqueness, nano Au particle can carry out Selective absorber to specific wavelength visible ray and present colourful color.Nm of gold material has special surface effect, quantum size effect and macro quanta tunnel effect, has the superior function that conventional material does not possess in electricity, magnetics, optics and chemical property.Therefore, have broad application prospects in catalysis, electronic material, micro element, reinforcing material and sensor material.Wherein surface-enhanced Raman character (the Surface enhanced Raman scattering of nano particle, SERS), the progress of local surface plasma resonance (Localized surface plasmon resonance, LSPR) aspect is rapid.
Local surface plasma resonance (LSPR) is when incident light beam strikes is to a kind of physical optics phenomenon produced during nanoparticle surface.When incident light frequency and metal free electron collective oscillation frequency occur to resonate, the resonant condition of LSPR is very responsive to the dielectric environment around nano particle, and macro manifestations produces strong absorption spectrum in specific wavelength coverage.Because LSPR phenomenon is produced by the light scattering of nano particle, therefore LSPR does not need traditional SPR(surface plasma body resonant vibration) light path system of the such complexity of technology, the research that can realize in bio-sensing, analytical chemistry, clinical medicine, biological detection etc. by simple, portable, sensitive fiber spectrometer.
Nano Au particle is difficult to play a role separately, must by the carrier of certain medium as particle.Using many is adopt glass substrate as substrate, and volume ratio is comparatively large, is difficult to the detection demand realizing microenvironment.Optical fiber has the characteristic of good transmission light, and capability of resistance to radiation is strong, affect little by extraneous factor, adopt optical fiber transmission signal can adapt to severe external environment, after thus using optical fiber to adopt chemical method to be assembled into optical fiber surface nano particle as substrate, acquisition testing signal has very strong actual application value.
At present, nano Au particle is combined with optical fiber and usually has following several mode: nano Au particle is modified at multimode optical fiber end face, nano Au particle is modified at optical fiber side and nano Au particle is modified in the airport of photonic crystal fiber.
KeitaMitsui (Applied Physics Letters, 85 (18): 4231 – 4233,2004) etc. people adsorbs last layer gold nano grain on fiber end face, adopt reflective optical fiber LSPR sensing arrangement, measure in real time the affinity of molecule, sensitivity reaches the level of conventional total reflection type SPR device.Stokes and Tuan Vo-Dinh (Sensors and ActuatorsB-Chemical, 69 (1-2): 28-36,2000) aluminum oxide nanoparticle and silver nano-grain are attached to optical fiber one end, real-time detection CFV (cresyl fast violet) molecule and BCB (brilliant cresyl blue) molecule in experiment, wherein the detection level of CFV molecule can reach 50ppb(1ppb=1 × 10
-6mg/ml).Viets (Joumal of RanmanSpectroscopy, 31 (7): 625-631,2000) successively proposes the optical fiber probe of angled end-face and tapered end face subsequently.The people such as LinTSaojen (Journal of Supercritical Fluids, 41 (2): 317-325,2007) adopt reflection type optical fiber LSPR sensor, under hyperbaric environment to liquid in Ni
2+concentration carries out monoclonal modification to the metallic particles be implanted on fiber end face again after having carried out test.The method that this class end face is modified, needs to use multimode optical fiber usually, and owing to adopting the mode of direct irradiation, general launching efficiency is not high.
Nano Au particle is modified at optical fiber side to need optical fiber lapping, corrode and draw cone process to fibre core or carry out, then modifies last layer metal nanoparticle, have an effect as the sensing unit of sensor and the external world.2000, Ni Weihai(Journalof Physical Chemistry C, 112 (22): 8105-8109,2008) etc. metal nano-rod is assembled in the optical fiber side be corroded by people, utilize evanscent field to encourage LSPR, obtain the sensitivity of scattering spectrum to ambient refractive index and reach 200nm/RIU.Tang(Sens.Actuators B, 119 (1): 105-109,2006) etc. people was coated onto long period fiber grating surface in 2006 nm of gold colloid, was used for detecting the change of ambient substance refractive index.This sensor can the concentration of detecting glucose, and when fixing deoxyribonucleoprotein (DNP) in nm of gold, accuracy of detection can reach 0.14mg/L.2011, the people such as Rani Dutta (AppliedOptics, E138-E144,2011) have studied the U-shaped optical fiber nanoparticle sensor made based on etch, owing to increasing the density of nano particle at optical fiber surface, observed the red shift in its absorption maximum region.The problem of this kind of sensor is when optical fiber is after the process of the method such as rubbing down, chemical corrosion, and it is very fragile that optical fiber becomes, and is easy to fracture.
The airport structure of photonic crystal fiber, gas and the good carrier of liquid in sensing, be used to design and produce nano Au particle sensor base, light transmits in Hollow-Core Photonic Crystal Fibers, light is limited in fibre core, analyzing thing is filled in airport, substantially increases the zone of action of light and SERS substrate like this.Nano Au particle is modified in the airport of photonic crystal fiber to be existed method complexity equally and is difficult to ensure conforming problem.
Generally speaking, nano Au particle sensor can be realized by above several method, but all has that launching efficiency is low, repeatability is not high and the shortcoming such as method is complicated.When using multimode optical fiber to carry out end face decorated nanometer gold particle, because the Lights section adopts the mode of direct irradiation, general launching efficiency is not high; When nano Au particle being modified at the side of optical fiber, because optical fiber is after the process of the method such as rubbing down, chemical corrosion, become very fragile, the repeatability of the nano Au particle sensor that this method is made is not high; Nano Au particle is modified in the airport of photonic crystal fiber to be existed method complexity equally and is difficult to ensure conforming problem.
Summary of the invention
The object of the present invention is to provide the nano Au particle sensor that a kind of structure is simple, volume is less, repeatability is high.The present invention also aims to the method for making that a kind of nano Au particle sensor is provided.
Nano Au particle sensor of the present invention comprises multi-core fiber, the end face of described multi-core fiber is frustum structure, total reflection film is coated with on frustum surface, the fiber end face being coated with total reflection film is fixed with the nano Au particle of rule arrangement, exciting light is injected in a fibre core of multi-core fiber, exciting light is reflected onto fiber end face place at frustum plated film place, and in fiber end face experiences total internal reflection, the local surface plasma resonance effect of the evanscent field excitation nano gold particle produced, reflected light is by collecting with the symmetrical moral fibre core of the fibre core injecting exciting light, by the change of reflected light spectrum perception external substance physical quantity.
Nano Au particle sensor of the present invention can also comprise:
The distributing position of multiple fibre cores of 1, described multi-core fiber is symmetrical about the optical fiber alignment of shafts, and is in same public covering.
The frustum structure of 2, described fiber end face is symmetrical circular cone structure or the polygonal wedge structure of symmetry.
3, the reflectance coating that described frustum surface is coated with is the one in metal film, full dielectric reflectance coating or electrolytic etching of metal matter reflectance coating.
The method for making of nano Au particle sensor of the present invention is:
The end face of the multi-core fiber of fibre core positional symmetry is processed into frustum shape, at frustum plated surface total reflection film, put into silane coupling A PTMS and methanol solution, at its surperficial fixed function group, described functional group is amino or coloured glaze base, put into nano Au particle colloidal sol, laser is passed in multi-core fiber, laser is reflected onto fiber end face place at frustum plated film place, and in fiber end face experiences total internal reflection, produce relevant evanscent field, under the effect of evanscent field near-field trapping, nano Au particle is fixed, take out optical fiber, and remove unnecessary nano Au particle colloidal sol by washed with de-ionized water, namely nano Au particle sensor is formed.
The method for making of nano Au particle sensor of the present invention can also comprise: in described nano Au particle colloidal sol, and nano Au particle particle can be the nanogold particle of spherical, bar-shaped, triangle, starlike or other patterns.
The present invention is based on following principle: the multi-core fiber end surface grinding of fibre core positional symmetry is become circular cone structure, and on the conical surface, plate one deck high reflectance total reflection film.As shown in Figure 4, the laser transmitted in fiber cores is reflexed to fiber end face at a certain angle by frustum offside reflection film, be totally reflected at fiber end face, although the energy of incident light wave is all reflected back optically denser medium when experiences total internal reflection, but in one deck that the interface of optically thinner medium is meagre, still there is energy, i.e. suddenly gesture ripple, produces the near-field trapping to nano Au particle thus.
Fig. 5 and Fig. 6 respectively show four-core fiber end face optical field distribution analogous diagram and twin-core fiber twin-beam and to be concerned with evanscent field standing wave.Multi-core fiber fibre core due to our use has symmetry and makes incident beam also have symmetry characteristic, the evanscent field that light beam produces will be formed in intersection point center interferes, capture region is divided into light and dark interference region, captured nano Au particle is at the move under influence of trapping stiffness, according to the arrangement that the distribution form of near field light gradient force potential well is orderly, thus complete optics self assembling process.Remove after being cured by nano Au particle and catch laser, in a core of multi-core fiber, pass to sense light, sense light goes out surface plasmons (LSPR) at the nanoscale gold particle surface excitation in total reflection district.
As shown in Figure 7, when light beam is radiated on spherical gold nanoparticles, oscillating electric field makes conduction electron one oscillates.When electron cloud has displacement relative to atomic nucleus, generation electrostatic restoring force is made conduction electron one oscillates by the Coulomb interactions between electronics and atomic nucleus.When the frequency of incident light is identical with intrametallic plasma oscillation frequency, will produce resonance, this resonance is macroscopically with regard to the absorption of exhibit metallic nano particle to light.The shape and size etc. of the density of its resonant frequency and electronics, electron effective mass, CHARGE DISTRIBUTION are closely related.
The resonant condition of LSPR is very responsive to the media environment around nano particle, and the material of particle ambient absorption will cause the red shift of LSPR resonant wavelength.According to Metal Ball extinction spectra formula:
Wherein, E(λ) be delustring amount, i.e. the summation of absorption and scattering; N is the local density of nano particle; A is the radius of metal nano spheroid; ε
outthat the specific inductive capacity of metal nano spheroid surrounding medium (is assumed to be arithmetic number, and uncorrelated with wavelength; For spheroid, ε
outfront coefficient χ value is 2); λ is incident wavelength; ε
iit is the imaginary part of metal nano spheroid specific inductive capacity; ε
rit is the real part of metal nano spheroid specific inductive capacity.
As the item (ε that resonates in denominator
r+ 2 ε
out) close to zero time, namely reach the resonant condition of LSPR.As can be seen from this model, the LSPR spectral characteristic of the metal nano spherical particles in extraneous dielectric environment depends on several aspect: the DIELECTRIC CONSTANT ε of environment residing for the radius a of nano particle, nano-particle material and nano particle
i, ε
rand ε
out.When the free electron metal that nano Au particle particle is desirable, ε
rcan by Drude model representation:
Wherein, γ is the frequency of fadings of metal, ω
outit is the frequency of incident light.ω
pbe the resonant frequency of metal, can be expressed from the next:
ω
p=(N'e
2/mε)
1/2（3）
Wherein, N' is free electron density, and m is electron mass, and ε is the specific inductive capacity of material relative vacuum.
Due at visible ray and ultraviolet light wave band, γ << ω
p, and during resonance, (ε
r+ 2 ε
out) → 0, simultaneously according to the relation (λ=2 π c/ ω) between wavelength and frequency, and the relation between refractive index and specific inductive capacity, formula (2) can be rewritten into
Wherein, λ
pthe resonant wavelength of metal, n
outit is metal nano spheroid ambient refractive index.
Time different by the medium refraction index of the known nano-scale gold particle sub-surface of formula (4), resonant positions (resonance angle or resonant wavelength) is by difference.Reflected light returns from symmetrical fibre core through end face reflection, then is received by spectrometer, is carried out the sensing of ambient substance refractive index by the observation measurement position of resonance peak or the change of intensity.
The present invention gives a kind of nano Au particle sensor and preparation method thereof.Multi-core fiber, near-field optical tweezers self-assembling technique are combined with nano Au particle local surface plasma resonance effect (LSPR), the near-field optical tweezers utilizing multi-core fiber to form is caught nano Au particle, make nano Au particle carry out optics self assembly regular array according to the capture region regularity of distribution, utilize end surface grinding technology to control the fiber end face of different cone angle and height to realize reflective local surface plasma resonance type optical fiber sensor.Multi-core fiber is utilized to be combined with nano Au particle, the volume of sensor can be reduced greatly, utilize evanscent field excited nano gold particle local surface plasma resonance effect (LSPR) that total reflection produces, overcome the shortcoming of conventional reflective sensor, effectively can improve the sensitivity of sensor, meanwhile, simple based on multi-core fiber nano Au particle self assembly sensor job operation, there is repeatability, for nano Au particle sensing technology provides a kind of effective method and technology.
Multi-core fiber, near-field optical tweezers self-assembling technique combine with nano Au particle local surface plasma resonance effect (LSPR) by the present invention, the near-field optical tweezers utilizing multi-core fiber to form can be caught nano Au particle, nano Au particle is made to carry out optics self assembly regular array according to the capture region regularity of distribution, achieve the new construction of nano Au particle sensor, have that structure is simple, less, the repeated advantages of higher of volume.
Accompanying drawing explanation
Fig. 1 is nano Au particle sensor one-piece construction schematic diagram.
Fig. 2 is nano Au particle sensor operating principles schematic diagram.
Fig. 3 is four-core fiber nano Au particle sensor construction schematic diagram.
Fig. 4 is that evanscent field of the present invention catches nano Au particle schematic diagram.
Fig. 5 is four-core fiber end face optical field distribution analogous diagram.
Fig. 6 is that twin-core fiber twin-beam is concerned with evanscent field standing wave.
Fig. 7 is the local surface plasma resonance schematic diagram of spherical gold nanoparticles.
Fig. 8 is the refraction index test system that nano Au particle Fibre Optical Sensor is formed.
Embodiment
Fig. 1 gives nano Au particle sensor one-piece construction.In figure, 1 is the multi-core fiber of distributing position about optical fiber alignment of shafts symmetry of multiple fibre core, and 2 is the multi-core fiber end face of frustum shape through processing, and 3 is total reflection film, and 4 for plating the multi-core fiber end face of reflectance coating, and 5 is nano Au particle.
Fig. 2 is nano Au particle sensor operating principles schematic diagram.In figure, 1 is the multi-core fiber of distributing position about optical fiber alignment of shafts symmetry of multiple fibre core, 2 for passing through the multi-core fiber end face of the frustum shape of processing, 3 is total reflection film, 4 for plating the multi-core fiber end face of reflectance coating, 5 is nano Au particle, and 6 is a fibre core of multi-core fiber, and 7 is sense light, 8 is reflected light to be measured, and 9 is the symmetrical fibre core with 6 symmetries.
Fig. 3 is four-core fiber nano Au particle sensor construction schematic diagram.In figure, 1 is the multi-core fiber of distributing position about optical fiber alignment of shafts symmetry of multiple fibre core, and 2 is the multi-core fiber end face of frustum shape through processing, and 3 is total reflection film, and 4 for plating the multi-core fiber end face of reflectance coating, and 5 is nano Au particle.
Fig. 8 is the refraction index test system that nano Au particle Fibre Optical Sensor is formed.In figure, 10 is light source, and 11 is circulator, and 12 is single-core fiber, and 13 is coupling mechanism, and 14 is multi-core fiber, and 15 nano Au particle optical fiber sensing probes for making, 16 is test substance solution, and 17 is spectrometer.
The present invention can realize in the following way:
Get the multi-core fiber 1 of one section of fibre core positional symmetry, utilize fiber cut technology fiber end face to be cut into plane perpendicular to shaft axis of optic fibre.Utilize optical fiber end grinding technology that fiber end face is processed into frustum shape 2, vacuum coating equipment is utilized to plate one deck high reflectance gold film 3 in fiber taper platform structure, optical fiber is put into silane coupling A PTMS and methanol solution, at its surperficial fixed function group (amino or coloured glaze base), optical fiber is put into nano Au particle colloidal sol, laser is passed in multi-core fiber, laser is reflected onto fiber end face place at frustum plated film place, and in fiber end face 4 experiences total internal reflection, produce relevant evanscent field, due to the effect of evanscent field near-field trapping, nano Au particle 5 is evenly arranged on fiber end face 4, after nano Au particle fixes, take out optical fiber, and take out unnecessary nano Au particle colloidal sol by washed with de-ionized water, namely nano Au particle sensor is formed.
The making of four-core fiber nano Au particle sensor, Fig. 3 is four-core fiber nano Au particle sensor construction schematic diagram.
1. the pre-service of optical fiber: get one section of four-core fiber, utilizes the coat of optical fiber wire-stripping pliers peeling optical fibre one end to be about 30mm, is cleaned up by fibre cladding with alcohol.
2. with optical fiber cutter, the part that optical fiber processing is crossed is cut, form smooth end face.
3. utilize optical fiber lapping technology optical fiber end to be ground to the frustum of a cone of α=36 °, the grinding degree of depth is 44.4 μm.
4. the gold-plated film of frustum of a cone end face utilizing vacuum coating technology step 3 to be ground.
5. the optical fiber after being processed by step 4 to be soaked in volume ratio be the concentration of 3:1 is the H of 96%
2sO
4with 30% H
2o
2middle immersion 30 minutes, clean surface.
6. by the optical fiber washed with de-ionized water after being processed by step 53 times, alcohol washes twice.
7. cleaned optical fiber to be immersed in the silane coupling A PTMS of volume tourney 1:10 and methanol solution 30 minutes.
8. by the optical fiber deionized water rinsing after being processed by step 73 times.
9. the optical fiber after being processed by step 8 is put into the nano Au particle colloidal sol of centrifugal mistake, exciting light is injected in a fiber cores, then produce the evanscent field formed by total internal reflection phenomena at fiber end face, due to the effect of evanscent field near-field trapping, nano Au particle is regularly arranged on fiber end face.
10. the optical fiber being fixed nano Au particle by step 9 is taken out, use washed with de-ionized water to take out unnecessary nano Au particle colloidal sol.
Utilize the refractive index of nano Au particle fiber sensor measuring different material.
Fig. 8 forms refraction index test system schematic for utilizing nano Au particle Fibre Optical Sensor.The light that light source 10 sends is coupled in single-core fiber 12 through circulator 11, the coupling power with multi-core fiber is realized through coupling mechanism 13 and multi-core fiber 14, the nano Au particle optical fiber sensing probe 15 made inserts in test substance solution 16, and reflected light returns by original route and detects reflectance spectrum by spectrometer 17.Can adopt modulation of source wavelength technology, realize the detection of resonant mode length scanning, the wavelength place of plasma resonance occurs, and will to there will be reflectivity minimum, measures its resonance wavelength reflected of different materials and will produce translation.Because the optical fiber frustum that total reflection occurs has certain angle of regulation range, also there is a scope in the incident light wave then producing resonance, therefore wide spectrum light source can be adopted to cause local surface plasma sub-resonance, the relation of output spectrum and wavelength is detected at the endpiece of optical fiber.
On the basis of theoretical research, use the fiber optic detection system built, the probe making different cone angle realizes the measurement of different material, by detecting the experiment such as refractive index, the identical refraction index solution test of heterogeneity, soluble protein Concentration Testing of the aqueous solution such as glucose, glycerine, the embody rule of research optical fiber nano Au particle self assembly sensor in biological detection.
Claims (7)
1. a nano Au particle sensor, comprise multi-core fiber, the end face of described multi-core fiber is frustum structure, it is characterized in that: be coated with total reflection film on frustum surface, the fiber end face being coated with total reflection film is fixed with the nano Au particle of rule arrangement, exciting light is injected in a fibre core of multi-core fiber, exciting light is reflected onto fiber end face place at frustum plated film place, and in fiber end face experiences total internal reflection, the local surface plasma resonance effect of the evanscent field excitation nano gold particle produced, reflected light is by collecting with the fibre core of the fibre core symmetry injecting exciting light, by the change of reflected light spectrum perception external substance physical quantity.
2. nano Au particle sensor according to claim 1, is characterized in that: the distributing position of multiple fibre cores of described multi-core fiber is symmetrical about the optical fiber alignment of shafts, and is in same public covering.
3. nano Au particle sensor according to claim 1 and 2, is characterized in that: the frustum structure of described fiber end face is symmetrical circular cone structure or the polygonal wedge structure of symmetry.
4. nano Au particle sensor according to claim 1 and 2, is characterized in that: the reflectance coating that described frustum surface is coated with is the one in metal film, full dielectric reflectance coating or electrolytic etching of metal matter reflectance coating.
5. the method for making of a nano Au particle sensor according to claim 1, it is characterized in that: the end face of the multi-core fiber of fibre core positional symmetry is processed into frustum shape, at frustum plated surface total reflection film, put into silane coupling A PTMS and methanol solution, at its surperficial fixed function group, put into nano Au particle colloidal sol, laser is passed in multi-core fiber, laser is reflected onto fiber end face place at frustum plated film place, and in fiber end face experiences total internal reflection, produce relevant evanscent field, under the effect of evanscent field near-field trapping, nano Au particle is fixed, take out optical fiber, and remove unnecessary nano Au particle colloidal sol by washed with de-ionized water, namely nano Au particle sensor is formed.
6. the method for making of nano Au particle sensor according to claim 5, is characterized in that: in described nano Au particle colloidal sol, and nano Au particle particle is spherical, bar-shaped, triangle or starlike nanogold particle.
7. the method for making of the nano Au particle sensor according to claim 5 or 6, is characterized in that: described functional group is amino or coloured glaze base.
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