CN109612970A - A kind of method and device enhancing gold nanosphere fluorescence intensity - Google Patents
A kind of method and device enhancing gold nanosphere fluorescence intensity Download PDFInfo
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- CN109612970A CN109612970A CN201811403930.6A CN201811403930A CN109612970A CN 109612970 A CN109612970 A CN 109612970A CN 201811403930 A CN201811403930 A CN 201811403930A CN 109612970 A CN109612970 A CN 109612970A
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N2021/6417—Spectrofluorimetric devices
Abstract
The invention belongs to nano materials and optical field.A method of enhancing gold nanosphere fluorescence intensity, continuous laser obtains gold nanosphere fluorescence in the gold nanoshell particles (4) that diameter is reunited for focusing excitation on the gold nanoshell particles (4) of 150-170 nanometers of reunion, gold nanosphere fluorescence enhances with the increase of laser irradiation time, best reinforcing effect is obtained when laser irradiation time reaches 4.5 seconds, is then weakened with the increase of laser irradiation time.The invention further relates to its devices that a kind of gold nanosphere reunited by continuous laser irradiation enhances its fluorescence intensity.The gold nanosphere that the present invention is reunited by the irradiation of near ultraviolet continuous laser makes adjacent gold nanosphere generate welding effect under the action of photo-thermal effect, and then generates extremely strong local surface etc. from enhancement effect, so that the fluorescence intensity of gold nanosphere enhances 150 times or more.
Description
Technical field
The invention belongs to nano material and optical field, specially a kind of gold nanosphere reunited by continuous laser irradiation
Enhance the method and device thereof of its fluorescence intensity.
Background technique
Noble metal nano particles, such as gold nanosphere, due to unique physicochemical properties, such as excellent photo-thermal spy
Property, splendid stability, biological non-toxicity, efficient catalysis characteristics and biocompatibility have it in numerous areas extensively
General application.Especially local surface possessed by gold nano grain etc. can greatly enhance and gold from enhancement effect
Nano particle closes on the linearity and non-linearity optic response of material (usually in 10 rans), has been used in surface increasing at present
Strong Raman spectrum, two-photon fluorescence, two frequencys multiplication the scientific researches and daily production such as acquisition in.
Gold nano grain itself also has single photon and two-photon fluorescence emission characteristics, this makes gold nano grain in biology
Imaging, the preparation of medical diagnosis and therapy and photoelectric device etc. have splendid application prospect.However, gold nano grain
Extremely low fluorescence quantum yield limits its extensive use in each field.In order to improve the amount of gold nano grain fluorescent emission
Sub- yield, most common method is induction enhancing of reuniting, i.e., by forming nanogold particle dimer, to enhance nanogold
Local surface of particle etc. improves fluorescent emission intensity from enhancement effect.Another kind enhancing gold nano grain fluorescence method be
Enhance the electronic state of gold nano grain highest occupied molecular orbital by the way that other suitable noble metals are added, to enhance visible
Optical transition improves quantum yield.These methods have some limitations, as dimer acquisition needs large scientific instrument
Accurate operation is carried out, it is expensive, it is complicated for operation, it is difficult to be used for industrial production；And other noble metals are added to gold nano
The reinforcing effect of grain fluorescence is limited, is typically only capable to the fluorescence intensity of gold nano grain increasing 20 times.
By the present invention in that the gold nanosphere reunited with continuous laser irradiation, makes gold nano based on its excellent Photothermal characterisation
Ball generates deformation, and welding effect is generated between adjacent gold nanosphere, and then extremely strong surface office is generated around pad
Domain etc. is greatly enhanced the fluorescence of gold nanosphere from enhancement effect.By the present invention in that with 405 nanometers of continuous lasers, it is right
Diameter is that 160 nanometers of gold nanosphere carries out continuous irradiation in 4.5 seconds, its fluorescence is made to have obtained 150 times or more of enhancing.This hair
Bright also achieve continuously adjusts gold nanosphere fluorescence spectrum.
Summary of the invention
Gold nano is quickly controllably realized by continuous laser the technical problems to be solved by the present invention are: how to provide one kind
The method and device thereof of ball fluorescence enhancement may be implemented to continuously adjust gold nanosphere fluorescence spectrum.
The technical scheme adopted by the invention is that: a method of enhancing gold nanosphere fluorescence intensity, continuous laser is straight
The gold nanoshell particles (4) that excitation is reunited are focused on the gold nanoshell particles (4) for the reunion that diameter is 150-170 nanometers obtains Jenner
Rice ball fluorescence, gold nanosphere fluorescence enhance with the increase of laser irradiation time, obtain when laser irradiation time reaches 4.5 seconds
Best reinforcing effect is obtained, is then weakened with the increase of laser irradiation time.
A kind of device enhancing gold nanosphere fluorescence intensity, including near ultraviolet continuous wave laser (1), dichroscope (2), object
Mirror (3), the gold nanoshell particles (4) reunited, coverslip (5), beam splitter (6), photodiode (7), spectrometer (8) are close purple
The gold nano for the reunion that the continuous laser that outer continuous wave laser (1) issues is 150-170 nanometers in diameter after object lens (3)
The gold nanoshell particles (4) that excitation is reunited are focused on ball particle (4) obtains gold nanosphere fluorescence；Gold nanosphere fluorescence passes back through
The fluorescence that object lens (3) form diverging afterwards is detected by photodiode (7) and spectrometer (8), photodiode (7) and spectrometer
(8) fluorescence detected enhances as laser irradiation time increases, and photodiode (7) and spectrometer (8) detect glimmering
Light starts to weaken after increasing to best reinforcing effect, and the fluorescence that photodiode (7) and spectrometer (8) detect is in laser irradiation
Maximum best reinforcing effect is obtained when time reaches 4.5 seconds.
As a kind of preferred embodiment: the preparation method of the gold nanoshell particles (4) of reunion is, is 0.005 by optical density (OD)
Diameter be 150-170 nanometers of gold nanosphere solution be spin-coated on the coverslip with a thickness of 0.17 millimeter, spin coating parameters are as follows: first
With revolving speed spin coating 10 seconds of 500 revs/min, then with revolving speed spin coating 20 seconds of 2000 revs/min, finally with 500 revs/min
Revolving speed spin coating 10 seconds, distance was 9-11 nanometers between gold nanosphere.
As a kind of preferred embodiment: the power of near ultraviolet continuous wave laser (1) is 2 milliwatts, the wave of the continuous laser of sending
A length of 405 nanometers, object lens (3) amplification factor is 100 times, numerical aperture 1.3.
Its principle of the invention are as follows: gold nanosphere has local surface etc. from enhancement effect, and gold nanosphere can be enhanced
Fluorescence intensity, reinforcing effect are influenced by gold nanosphere surface roughness.Pass through chemically synthesized gold nanosphere, surface phase
To smooth, therefore reinforcing effect is weaker.When continuous laser irradiates gold nanosphere, due to the photothermal conversion effect that gold nanosphere is excellent
Fruit makes it be rapidly heated, and surface is caused to melt, and then deformation occurs.After adjacent gold nanosphere melts, contact with each other to form point
Sharp pad, and then extremely strong local surface of generation etc. significantly enhances the fluorescence intensity of gold nanosphere from enhancement effect.
The beneficial effects of the present invention are: the gold nanosphere that the present invention is reunited by the irradiation of near ultraviolet continuous laser, makes adjacent
Gold nanosphere generates welding effect under the action of photo-thermal effect, and then extremely strong local surface of generation etc. makes from enhancement effect
The fluorescence intensity for obtaining gold nanosphere enhances 150 times or more.Compared to the existing method for forming gold nanosphere dimer, this method tool
There is low in cost, simple process, be suitable for large area industrial operation.Compared to the other noble metal nano particles of addition
Method, the present invention have more preferably fluorescence enhancement effect.The present invention efficiently solves the problems, such as that gold nanosphere fluorescence efficiency is low,
Allow the gold nanosphere with hyperfluorescence emissivities apply bio-imaging, in terms of, improve
The clarity of imaging and the accuracy of diagnosis, enhance the effect for the treatment of.Compared to gold nanosphere dimer or it is added other expensive
Metal nanoparticle fixed fluorescence enhancement effect obtained, the present invention is to the reinforcing effect of gold nanosphere fluorescence with irradiation time
And change, irradiation can be stopped according to actual needs when obtaining required fluorescence intensity.Therefore, the present invention is glimmering to gold nanosphere
The enhancing of light has greater flexibility, and application range is wider, can select to use according to the actual situation.Using continuous laser
While irradiation reunion gold nanosphere enhances its fluorescence intensity, the fluorescence spectrum of gold nanosphere also changes therewith, fluorescence light
The degree of spectrum variation depends on the time of continuous laser irradiation.Therefore it can obtain with the gold nanosphere fluorescence light continuously adjusted
Spectrum, in terms of have important application.
Detailed description of the invention
Fig. 1 is a kind of apparatus structure schematic diagram for enhancing gold nanosphere fluorescence intensity of the present invention；
Fig. 2 is that the transmission electron microscope(TEM) of the gold nanosphere sample prepared by spin coating characterizes；
Fig. 3 is that 405 nanometers of continuous lasers irradiate the fluorescence intensity of lower gold nanosphere with the variation relation figure of irradiation time；
Fig. 4 is that 405 nanometers of continuous lasers irradiate the fluorescence enhancement multiple of lower gold nanosphere with the variation relation figure of irradiation time；
Fig. 5 is that 405 nanometers of continuous lasers irradiate the fluorescence spectrum of lower gold nanosphere and spectrum peak position is closed with the variation of irradiation time
System's figure；
In figure: 1- near ultraviolet continuous wave laser, 2- dichroscope, 3- object lens, the gold nanosphere that 4- reunites, 5- coverslip, 6- points
Shu Jing, 7- photodiode, 8- spectrometer.
Specific embodiment
As shown in Figure 1, the device of one of the present embodiment enhancing gold nanosphere fluorescence intensity, including 1- laser, 2-
Dichroscope, 3- object lens, the gold nanosphere that 4- reunites, 5- coverslip, 6- beam splitter, 7- photodiode, 8- spectrometer.It is described
Laser 1 is the continuous wave laser that wavelength is 405 nanometers, and the dichroscope 2 is on the emitting light path of laser 1, for anti-
Laser is penetrated into object lens 3, the object lens 3 are located on the reflected light path of dichroscope 2；The object lens 3 while focusing laser,
Collect the fluorescence that is issued by reunion gold nanosphere 4, generated Fluoroscopic crosses dichroscope 2 and is transmitted to beam splitter 6, and described point
For beam mirror 6 on the transmitted light path of dichroscope 2, the reflected light path and transmitted light path of the dichroic 2 are contrary；By gold of reuniting
The fluorescence that nanosphere 4 generates is detected by photodiode 7 and spectrometer 8, two pole of photoelectricity respectively by 6 beam splitting of beam splitter
Pipe 7 is on the transmitted light path of beam splitter 6, and the spectrometer 8 is on the reflected light path of beam splitter 6, the transmitted light of the beam splitter 6
Road and reflected light path are at right-angle relationship.
The operating power of the laser 1 is 2 milliwatts.
The dichroscope 2 may be implemented to be greater than the saturating of 420 nano fluorescents to the reflection of 405 nanometer lasers and wavelength
It penetrates.
The amplification factor of the object lens 3 is × 100, and numerical aperture is NA=1.3.
The beam splitter 6 is 1:9 to the splitting ratio of fluorescence, wherein weaker fluorescence is located on transmitted light path, it is stronger glimmering
Light is located on reflected light path.
The photodiode 7 for observing the fluorescence intensity of gold nano in real time.
The spectrometer 8 for acquiring the fluorescence spectrum of gold nanosphere in real time.
Embodiment 2
The method of one of the present embodiment enhancing gold nanosphere fluorescence intensity, comprising the following steps:
1) the gold nanosphere sample 4 that preparation is reunited:
A piece of coverslip is taken, is cleaned respectively with acetone, potassium hydroxide and deionized water, is revolved gold nanosphere solution by spin-coating method
It applies on the cover slip, prepares the gold nanosphere sample of reunion.
The cover-glass thickness is 0.17 millimeter.
The gold nanosphere is prepared by seed mediating growth method, and gold nanosphere diameter obtained is about 160 nanometers,
The optical density (OD) of gold nanosphere solution used in spin coating is 0.005.
The design parameter of the spin-coating method are as follows: 1. first with revolving speed spin coating 10 seconds of 500 revs/min；2. then with 2000
Rev/min revolving speed spin coating 20 seconds；3. finally with revolving speed spin coating 10 seconds of 500 revs/min.
Fig. 2 gives the transmission electron microscope characterization result of prepared reunion gold nanosphere sample, it can be found that view
The a large amount of gold nanosphere in Yezhong is reunited together, and the diameter of each gold nanosphere is between 160 rans, adjacent gold nanosphere
Spacing in 10 rans, gold nanosphere is dispersed in coverslip surface well, and gold nanosphere is in the side perpendicular to coverslip
It does not stack upwards.
2) gold nanosphere 4 reunited using 405 nanometers of irradiations of continuous laser 1:
405 nanometers of continuous wave lasers 1 are opened, laser power is adjusted to 2 milliwatts；Laser emitting direction is adjusted, object is passed through
Mirror.Photodiode 7 is opened, distance of the coverslip 5 relative to object lens 3 is adjusted, the signal that observation photodiode 7 exports is strong
Degree, when signal strength reaches maximum, illustrates the gold nanosphere surface that laser has focussed on coverslip.
3) gold nanosphere fluorescence intensity is observed, gold nanosphere fluorescence spectrum is acquired:
Photodiode 7 and spectrometer 8 are opened, in the case where laser has focused on gold nanosphere surface, observation is received with 405
Rice continuous laser irradiation, the fluorescence intensity of gold nanosphere and the variation of fluorescence spectrum.
Fig. 3 gives what photodiode detected, under 405 nanometers of continuous laser irradiations, the fluorescence intensity of gold nanosphere
With the variation track of irradiation time.It can be seen from the figure that in first 0.5 second of 405 nanometers of continuous lasers irradiation, gold nanosphere
Fluorescence intensity there is no a significant change, stablize 0.55 × 104A (fluorescent photon)/second；The fluorescence intensity of subsequent gold nanosphere
It is remarkably reinforced, and with the increase of irradiation time, fluorescence is more and more stronger；At 4.5 seconds, fluorescence intensity reached maximum, and about 8.5
×105A/second；With the further irradiation of 405 nanometers of continuous lasers, certain attenuation trend is presented in the fluorescence of gold nanosphere；
After the 405 nanometers of continuous lasers of closing in 5.35 seconds, the fluorescence of gold nanosphere is also immediately turned off.
In order to further illustrate the fluorescence enhancement effect of gold nanosphere, the defined herein fluorescence enhancement factor are as follows: 405 nanometers of companies
Continuous laser irradiationtAfter time, the ratio of fluorescence intensity and initial fluorescent intensity.Fig. 4 gives the fluorescence enhancement of gold nanosphere
The factor with 405 nanometers of continuous laser irradiation times variation.It can be seen from the figure that 1 after 405 nanometers of continuous lasers irradiate
Between second to 4 seconds, rapid growth is presented in the fluorescence intensity of gold nanosphere: after laser irradiation 2 seconds, the fluorescence intensity of gold nanosphere
Increase 30 times or more；After irradiation 3 seconds, fluorescence intensity increases 90 times or more；After irradiation 4 seconds, fluorescence intensity increase is connect
Nearly 150 times.During 4 seconds to 5 seconds of laser irradiation, fluorescence intensity is relatively stable, then shows certain decaying.
Further, with the enhancing of gold nanosphere fluorescence intensity, significant change also occurs for fluorescence spectrum.Fig. 5 a is provided
After 405 nanometers of continuous lasers irradiation different times, the fluorescence spectrum of gold nanosphere；It can be found that with the increasing of irradiation time
Long, fluorescence wave crest (fluorescence spectrum most strength) is mobile to long wavelength.Fig. 5 b gives fluorescence wave crest with the variation of irradiation time；It can
To find irradiation time during 0 second to 3 seconds, fluorescence wave crest is gradually increased to 710 nanometers from 645 nanometers of beginning；When irradiation
Between during 3 seconds to 5 seconds, fluorescence crest location is basically unchanged.
Claims (3)
1. a kind of method for enhancing gold nanosphere fluorescence intensity, it is characterised in that: continuous laser is 150-170 nanometers in diameter
The gold nanoshell particles (4) that excitation is reunited are focused on the gold nanoshell particles (4) of reunion obtains gold nanosphere fluorescence, gold nanosphere
Fluorescence enhances with the increase of laser irradiation time, and best reinforcing effect is obtained when laser irradiation time reaches 4.5 seconds, with
Weaken afterwards with the increase of laser irradiation time.
2. it is a kind of enhance gold nanosphere fluorescence intensity device, it is characterised in that: including near ultraviolet continuous wave laser (1), two to
Look mirror (2), object lens (3), the gold nanoshell particles (4) reunited, coverslip (5), beam splitter (6), photodiode (7), spectrum
Instrument (8), the reunion that the continuous laser that near ultraviolet continuous wave laser (1) issues is 150-170 nanometers in diameter after object lens (3)
Gold nanoshell particles (4) on focus excitation reunite gold nanoshell particles (4) obtain gold nanosphere fluorescence；Gold nanosphere fluorescence
Pass back through object lens (3) and form the fluorescence of diverging afterwards and detected by photodiode (7) and spectrometer (8), photodiode (7) and
The fluorescence that spectrometer (8) detects enhances as laser irradiation time increases, photodiode (7) and spectrometer (8) detection
To fluorescence increase to after best reinforcing effect and start to weaken, the fluorescence that photodiode (7) and spectrometer (8) detect is swashing
Maximum best reinforcing effect is obtained when light irradiation time reaches 4.5 seconds.
3. a kind of device for enhancing gold nanosphere fluorescence intensity according to claim 1, it is characterised in that: the Jenner of reunion
Rice ball particle (4) preparation method be 150-170 nanometers of gold nanosphere solution spin coatings by the diameter that optical density (OD) is 0.005
On the coverslip with a thickness of 0.17 millimeter, spin coating parameters are as follows: first with revolving speed spin coating 10 seconds of 500 revs/min, then with
2000 revs/min of revolving speed spin coating 20 seconds, finally with revolving speed spin coating 10 seconds of 500 revs/min, distance is 9- between gold nanosphere
11 nanometers.
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| CN109596584A (en) * | 2018-11-28 | 2019-04-09 | 山西大学 | A kind of method and device enhancing gold nanosphere fluorescence intensity |
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