CN107267940B - A kind of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate and its application - Google Patents
A kind of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate and its application Download PDFInfo
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- CN107267940B CN107267940B CN201710431891.XA CN201710431891A CN107267940B CN 107267940 B CN107267940 B CN 107267940B CN 201710431891 A CN201710431891 A CN 201710431891A CN 107267940 B CN107267940 B CN 107267940B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- 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
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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Abstract
The invention discloses a kind of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate and its applications, will be spare after glass slide cleaning, drying；Au-Cu and Ag-Al composition target is separately mounted on DC cathode, the glass slide after cleaning is packed into sample stage, booting, it vacuumizes, then leads to people's argon gas, open shielding power supply, alternating sputtering Au-Cu and Ag-Al, sputtering is completed, and shielding power supply is closed, and stops ventilation, close molecular pump, powered-down source is cooled to room temperature under natural vacuum, then takes out sample.The film surface enhancing fluorescent base bottom that operation of the present invention is simple, environmental-friendly, deposition velocity is fast, high-efficient, production cost is low, is easy to produce in batches, the film is multilayered structure, by on glass alternating deposit Au-Cu and Ag-Al prepare, the instrument of use is common magnetic control sputtering device.
Description
Technical field
The invention belongs to field of spectroscopy more particularly to a kind of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrates
And its application.
Background technique
Fluorescent technique is as a kind of important modern spectral technique, and with high sensitivity, easy to operate, detection is rapid, nothing
The advantages that needing sample pre-treatments, meets the needs of real time on-line monitoring, is therefore widely used in the inspection of the environment such as atmosphere, water body
It surveys.Polycyclic aromatic hydrocarbon is pollutant generally existing in water environment, has the characteristics that inertia is relatively strong, more stable, difficult to degrade, in reality
In use, even if the content of polycyclic aromatic hydrocarbon is few in water body, but when used for a long time since its cumulative effect can still generate human body
The harm such as carcinogenic, the rugged, mutagenesis of cause.Therefore, prediction more early to the polycyclic aromatic hydrocarbon pollutant in water environment more can be avoided timely
Its harmfulness, this puts forward new requirements the detection sensitivity of fluorescent technique.
There are many ways to for improving fluorescence detection sensitivity, such as: the inspection of instrument is improved using new technology, new device
Survey sensitivity;Long wavelength's probe molecule is selected to reduce the interference of background fluorescence;It is anti-using enzyme linked immunoassay, polymerase chain
Answer, the biochemical methods such as more fluorescent chromophore probes improve the amplification factor of fluorescence signal, etc..But these methods improve
The detection sensitivity limitation of fluorescent technique is very big, and the degree of raising is limited by the quantum yield of fluorescence species itself, photodissociation
And interference of background fluorescence etc..From the aspect of improving instrument, although being reduced to the maximum extent in strict control experiment condition
In the case where background fluorescence, it may be implemented to monomolecular measurement, but this measurement needs to use complicated optical system, to inspection
The quality requirement for surveying device is also especially high, therefore instrument price is expensive, and experimentation requires that strictly, this method popularization and application are deposited
In Difficulty.Therefore, it is necessary to find the approach of new raising fluorescence detection sensitivity.
In the 1970s, the discovery precious metal surface such as Drexhage has important shadow to the fluorescence property of neighbouring fluorogen
It rings, the plasma oscillation and electromagnetic field of metal surface cut effect, make to be distributed in glimmering near metal surface or sol particle
The fluorescent emission intensity of light object enhances than free state, i.e. surface-enhanced fluorescence effect.Maryland university, the U.S.
It is plentiful and substantial that professor Lakowiczpsj leads its research team to achieve in the experiment and theoretical research of surface-enhanced fluorescence effect
Achievement, raised the new page of surface-enhanced fluorescence effect study.Be currently used for fluorescent surface enhancing substrate be typically all
Using the simple substance golden film or silverskin of chemical reduction method preparation, the fluorescence of very close limit can only be enhanced, and deposit
Cannot accurately control in deposition rate, membrane-film preparation process environmental pollution the problems such as.Harbin Institute of Technology Sun Xiudong is taught theoretically
The prediction surface plasmon polariton of each layer and local surface phasmon in multi-layer film structure intercouple and may be implemented
Fluorescence is further enhanced, and relevant experimental study has not been reported.
Summary of the invention
The object of the present invention is to provide a kind of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrates.
To achieve the goals above the present invention adopts the following technical scheme:
A kind of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate, which is characterized in that preparation method includes following
Step:
It 1) will be spare after glass slide cleaning, drying；
2) Au-Cu and Ag-Al composition target being separately mounted on DC cathode, the glass slide after cleaning is packed into sample stage,
The distance for adjusting target and substrate is 48-52mm；
3) it is switched on, is evacuated to 0.9-1.1x10-3Pa, then leads to people's argon gas, and adjustment Ar flow is 29-31sccm, adjustment
Operating air pressure is to 1.4-1.6Pa；
4) shielding power supply is opened, alternating sputtering Au-Cu and Ag-Al, wherein sputtering power is respectively 40W and 60W, and control is single
Secondary sputtering time is 0.9-1.1min, and total sputtering time is 5.9-6.1min；
5) it sputters and completes, close shielding power supply, stopping is ventilated, pass molecular pump, powered-down source, is cooled to room under natural vacuum
Temperature then takes out sample.
A kind of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate, it is characterised in that: preparation method packet
Include following steps:
It 1) will be spare after glass slide cleaning, drying；
2) Au-Cu and Ag-Al composition target being separately mounted on DC cathode, the glass slide after cleaning is packed into sample stage,
The distance for adjusting target and substrate is 50mm；
3) it is switched on, is evacuated to 1x10-3Then pa leads to people's argon gas, adjustment Ar flow is 30sccm, and adjustment operating air pressure is extremely
1.5Pa；
4) shielding power supply is opened, alternating sputtering Au-Cu and Ag-Al, wherein sputtering power is respectively 40W and 60W, and control is single
Secondary sputtering time is 1min, and total sputtering time is 6min；
5) it sputters and completes, close shielding power supply, stopping is ventilated, pass molecular pump, powered-down source, is cooled to room under natural vacuum
Temperature then takes out sample.
A kind of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate, it is characterised in that: Au-Cu and Ag-
Au/Cu mass ratio=1/4, Ag/Al mass ratio=2/3 in Al composition target.
The application of the Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate, which is characterized in that it can be mentioned
Fluorescence detection sensitivity in high modern times spectral technique.
Beneficial effects of the present invention: operation of the present invention is simple, environmental-friendly, deposition velocity is fast, high-efficient, production cost
Bottom, the film surface enhancing fluorescent base bottom for being easy to produce in batches, which is multilayered structure, passes through the alternating deposit on glass
Au-Cu and Ag-Al preparation, the instrument of use is common magnetic control sputtering device.The present invention can make full use of different in composite membrane
Metal and the multiple layering effect, that is, surface plasmon-polarition and local surface phasmon of multilayer film intercouple to realize width
The surface enhanced of spectral limit fluorescence.
Detailed description of the invention
Fig. 1 is that embodiment STEM sectional view shows that prepared film is multilayered structure, and thickness in monolayer is controllable in 2-4nm；
Fig. 2 is that embodiment utilizes common glass slide, monofilm, multilayer film respectively to the fluorescence after phenanthrene, pyrene, anthracene fluorometric investigation
Strength Changes.
Specific embodiment
A kind of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate, preparation method the following steps are included:
It 1) will be spare after glass slide cleaning, drying.
2) Au-Cu and Ag-Al composition target being separately mounted on DC cathode, the glass slide after cleaning is packed into sample stage,
The distance for adjusting target and substrate is 50mm.Au/Cu mass ratio=1/4, Ag/Al mass ratio=2/ in Au-Cu and Ag-Al composition target
3。
3) it is switched on, is evacuated to 1x10-3Then pa leads to people's argon gas, adjustment Ar flow is 30sccm, and adjustment operating air pressure is extremely
1.5Pa。
4) shielding power supply is opened, alternating sputtering Au-Cu and Ag-Al, wherein sputtering power is respectively 40W and 60W, and control is single
Secondary sputtering time is 1min, and total sputtering time is 6min.
5) sputtering is completed, and closes shielding power supply, stops ventilation, closes molecular pump, powered-down source.Room is cooled under natural vacuum
Temperature then takes out sample.
A kind of application of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate, can be improved modern spectrum skill
Fluorescence detection sensitivity in art.
The performance test of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate: as shown in Figure 1 and Figure 2；
The test of STEM Cross Section Morphology shows that prepared film substrate is multilayered structure, and every layer of thickness is about 2-4 nm, always
Thickness is about 25nm, to three kinds of differences when fluorometric investigation shows to do surface fluorescence enhancing substrate using monofilm Au-Cu, Ag-Al
Phenanthrene, pyrene, anthracene the fluorescence enhancement factor be respectively 4,1.5,3 and 2,5,2, and when using multilayer film fluorescence enhancement substrate
The fluorescence enhancement factor be respectively 9,7,8, i.e., Au-Cu/Ag-Al nano-multilayer film is a kind of very effective surface-enhanced fluorescence
Substrate.
Claims (3)
1. a kind of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate, it is characterised in that: preparation method includes following step
It is rapid:
It 1) will be spare after glass slide cleaning, drying；
2) Au-Cu and Ag-Al composition target is separately mounted on DC cathode, the glass slide after cleaning is packed into sample stage, adjustment
The distance of target and substrate is 50mm；
3) it is switched on, is evacuated to 1x10-3Then pa leads to people's argon gas, adjustment Ar flow is 30sccm, and adjustment operating air pressure is extremely
1.5Pa；
4) shielding power supply is opened, alternating sputtering Au-Cu and Ag-Al, wherein sputtering power is respectively 40W and 60W, and control single splashes
Penetrating the time is 1min, and total sputtering time is 6min；
5) it sputters and completes, close shielding power supply, stopping is ventilated, pass molecular pump, powered-down source, is cooled to room temperature under natural vacuum, so
After take out sample, preparation-obtained film substrate is nano-multilayered structures, every layer with a thickness of 2-4 nm, overall thickness is about
25nm。
2. a kind of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate according to claim 1, feature exist
In: Au/Cu mass ratio=1/4, Ag/Al mass ratio=2/3 in Au-Cu and Ag-Al composition target.
3. a kind of application of Au-Cu/Ag-Al nano-multilayer film surface-enhanced fluorescence substrate as described in claim 1, feature
It is, the fluorescence detection sensitivity in modern spectral technique can be improved.
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| CN109487221B (en) * | 2018-12-12 | 2021-04-02 | 中国科学院合肥物质科学研究院 | Ag-Au-Al-Cr-Cu nano composite film surface enhanced fluorescent substrate and preparation method thereof |
| CN115181953B (en) * | 2022-09-09 | 2022-12-06 | 清华大学 | Preparation method of surface plasmon thin film and method for preparing multilayer film metamaterial |
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| CN102965538A (en) * | 2012-11-10 | 2013-03-13 | 清华大学 | Polycrystalline silver platinum alloy plasma thin-film material and preparation method thereof |
| CN103353451A (en) * | 2013-07-04 | 2013-10-16 | 首都师范大学 | Preparation method of nano probe |
| CN104060245A (en) * | 2014-06-10 | 2014-09-24 | 上海交通大学 | Super-hydrophobic nano-silver raman-enhanced substrate material and preparation method thereof |
| CN104280376A (en) * | 2013-07-10 | 2015-01-14 | 任贻均 | Surface enhanced Raman spectroscopy (SERS) sensing substrate and manufacturing method thereof |
| CN104372299A (en) * | 2013-09-23 | 2015-02-25 | 中国科学院合肥物质科学研究院 | Multilayer-structural hard wear-resistant lubrication coating and preparation method thereof |
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| US8836941B2 (en) * | 2010-02-10 | 2014-09-16 | Imra America, Inc. | Method and apparatus to prepare a substrate for molecular detection |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776536A (en) * | 2011-05-12 | 2012-11-14 | 中国科学院合肥物质科学研究院 | Mercapto-beta-cyclodextrin modified silver nano-rode array, its preparation method and its use |
| CN102965538A (en) * | 2012-11-10 | 2013-03-13 | 清华大学 | Polycrystalline silver platinum alloy plasma thin-film material and preparation method thereof |
| CN103353451A (en) * | 2013-07-04 | 2013-10-16 | 首都师范大学 | Preparation method of nano probe |
| CN104280376A (en) * | 2013-07-10 | 2015-01-14 | 任贻均 | Surface enhanced Raman spectroscopy (SERS) sensing substrate and manufacturing method thereof |
| CN104372299A (en) * | 2013-09-23 | 2015-02-25 | 中国科学院合肥物质科学研究院 | Multilayer-structural hard wear-resistant lubrication coating and preparation method thereof |
| CN104060245A (en) * | 2014-06-10 | 2014-09-24 | 上海交通大学 | Super-hydrophobic nano-silver raman-enhanced substrate material and preparation method thereof |
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