CN105755431A - Preparation method for synthesizing gold nanoparticle-coated SERS substrate on basis of replacement method - Google Patents
Preparation method for synthesizing gold nanoparticle-coated SERS substrate on basis of replacement method Download PDFInfo
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- CN105755431A CN105755431A CN201610261432.7A CN201610261432A CN105755431A CN 105755431 A CN105755431 A CN 105755431A CN 201610261432 A CN201610261432 A CN 201610261432A CN 105755431 A CN105755431 A CN 105755431A
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
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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
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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Abstract
The invention provides a preparation method for synthesizing a gold nanoparticle-coated SERS substrate on the basis of a metal replacement method.The preparation method comprises the steps that a zinc film is plated on the surface of a slide through a vacuum magnetron sputtering technique, then the slide is soaked in low-concentration chloroauric acid sol, gold nanoparticles are uniformly adsorbed on a slide substrate through the method of replacing chloroautic acid with zinc, and the repeatable SERS substrate which has a high enhancing factor on rhodamine is prepared.The SERS active substrate prepared through the preparation method has the advantages that the preparation technology is simple and easy to operate, the repeatability is high, and the enhancing factor is large, and the detection limit of the SERS substrate on rhodamine can reach 10<-7>.
Description
Technical field
The present invention relates to applications to nanostructures field, in particular it relates to one synthesizes gold nano based on displacement method
The SERS substrate preparation method of grain.
Background technology
From surface enhanced Raman scattering effect (SERS) find since by people be applied to environment measuring, chemical analysis,
The numerous areas such as biological medicine.In the past few decades, a focus of the preparation of SERS substrate always people's research.
In general, the enhancing of Raman signal needs there are the metal nanostructures such as certain orderly Jin Jin above base, such as nanometer
Ball, nanometer rods, island nanostructured etc..
Nanostructured needed for preparing SERS base has multiple method, as directly utilized magnetic control sputtering system by gold, silver
Etc. sputtering on slide base, form SERS substrate [Li J, Fang Y.An investigation of the surface
enhanced Raman scattering(SERS)from a new substrate of silver-modified silver electrode
by magnetron sputtering[J].Spectrochimica Acta Part A:Molecular and Biomolecular
Spectroscopy, 2007,66 (4): 994-1000.], but the SERS base particle skewness that this type of method is prepared,
Granular size is inconsistent, wayward, and roughness is also inadequate, affects repeatability and the focus quantity of SERS,
Thus affect SERS effect.
Summary of the invention
One of the problem existed for above-mentioned prior art/, the present invention provides a kind of based on displacement method synthesis gold nano grain
SERS substrate preparation method, even particle distribution, add the quantity of SERS substrate surface activity focus, enter one
Step improves Raman signal sensitivity.
For realizing above-mentioned purpose, the present invention by the following technical solutions: the inventive method is by carrying out magnetic to surface of glass slide
Control sputter coating, forms the nano thin-film of zinc, then by the method for displacement chlorauric acid solution in substrate in surface of glass slide
Form gold nano grain, make repeatably, have the SERS substrate of high enhancer.
Concrete, the present invention provides a kind of SERS substrate preparation method based on displacement method synthesis gold nano grain,
Described method comprises the steps:
Step 1: slide is sequentially placed into ultrasonic cleaning in acetone and alcohol, takes out after cleaning up by deionized water；
Step 2: put in magnetron sputtering coater by the slide cleaned, forms zinc nano thin-film on slide；
Step 3: the slide after the plated film of step 2 gained is put into stirring reaction in chlorauric acid solution, is formed and adhere to table
The nano particle in face；
Step 4: the Wafer Cleaning that step 3 reacted also is dried, standby.
Preferably, in described step 2, including:
Step 2.1: the vacuum of magnetron sputtering coater inner chamber is reached 10-5～10-4After Pa, zinc target power output is fixed on
30～50W, set plated film time 20-200s；
Step 2.2: start sputtering system, starts plated film.
Preferably, in described step 3, including:
Step 3.1: the slide being coated with zinc film is put in the chlorauric acid solution that molar concentration is 0.01～0.1mmol/L,
Soak 5-30 minute at 30～35 DEG C；
Step 3.2: taken out by slide, first with alcohol washes, then cleans by deionized water, standby after natural drying.
Preferably, in described step 4, the silicon chip substrate deionized water prepared is cleaned 2～3 times, natural drying
Final vacuum preserves, standby.
The present invention uses magnetron sputtering coating system to form the zinc nano thin-film of densification, this nano thin-film microcosmic in surface of glass slide
Structure is the island structure of flake nano zinc composition.Then form gold nano grain by displacement method and adsorb at slide table
Face, just obtains a kind of preferably SERS substrate after natural drying.The present invention directly passes through magnetron sputtering in solid substrate
Plated film also directly generates metal Nano structure by displacement reaction.The size of gold nano grain, spacing, pattern can pass through
The concentration of regulation plated film time, reaction time and gold chloride regulates and controls.Substrate prepared by the method is glued due to gold nano grain
Attached ratio is stronger, the most reliable and the most stable, repeatable high, and preparation means is simple, is quick on the draw, and has the biggest answering
Use prospect.
Compared with prior art, the present invention has a following improvement effect:
(1) with existing directly do SERS substrate by gold-plated on slide base, Ag films compared with, the present invention is
Big innovative point is: uses zinc nano thin-film, makes substrate surface pattern more coarse by further displacement method,
Granule-morphology is the most complicated, adds the quantity of SERS substrate surface activity focus, improves Raman letter further
Number sensitivity；
(2) the technology of the present invention preparation method is simple, and preparation process controllability is strong；
(3) the SERS substrate surface gold nano grain adhesiveness that prepared by the present invention is very strong, difficult drop-off；
(4) detection of rhodamine (R6G) is limited and reaches 10 by the SERS substrate that prepared by the present invention-7Mol/L, SERS
Respond well.
Accompanying drawing explanation
The detailed description made non-limiting example with reference to the following drawings by reading, other of the present invention is special
Levy, purpose and advantage will become more apparent upon:
Fig. 1 is the stereoscan photograph of SERS substrate surface gold nano grain in the embodiment of the present invention, wherein: (a)
Stereoscan photograph for SERS substrate surface gold nano grain in embodiment 1；B () is in example 2
The stereoscan photograph of SERS substrate surface gold nano grain；
Fig. 2 be concentration be 10-7Mol/L rhodamine (R6G) is prepared suprabasil in embodiment 1,2,3 and 4
Strengthen Raman spectrogram.
Detailed description of the invention
Below in conjunction with specific embodiment, technical solution of the present invention is further described.Following example will assist in this area
Technical staff is further appreciated by the present invention, but limits the present invention the most in any form.It should be pointed out that, to this area
For those of ordinary skill, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement.These
Broadly fall into protection scope of the present invention.
Embodiment 1
The present embodiment provides a kind of SERS substrate preparation method based on displacement method synthesis gold nano grain, described side
Method comprises the steps:
A: slide is sequentially placed into ultrasonic cleaning 5 minutes in acetone and alcohol, takes out after cleaning up by deionized water；
B: the vacuum of magnetron sputtering coater inner chamber is reached 10-5After Pa, zinc target power output is fixed on 50W, sets
Plated film time 20s；
C: start sputtering system, starts plated film；
D: the slide after the plated film of step c gained is put in the chlorauric acid solution that molar concentration is 0.01mmol/L, 30 DEG C
Lower immersion 5 minutes；
F: taken out by slide, first with alcohol washes, then cleans 2-3 time by deionized water, standby after natural drying.
Embodiment 2
The present embodiment provides a kind of SERS substrate preparation method based on displacement method synthesis gold nano grain, described side
Method comprises the steps:
A: slide is sequentially placed into ultrasonic cleaning 5 minutes in acetone and alcohol, takes out after cleaning up by deionized water；
B: the vacuum of magnetron sputtering coater inner chamber is reached 10-4After Pa, zinc target power output is fixed on 30W, sets
Plated film time 50s；
C: start sputtering system, starts plated film；
D: the slide after the plated film of step c gained is put in the chlorauric acid solution that molar concentration is 0.05mmol/L, 30 DEG C
Lower immersion 5 minutes；
F: taken out by slide, first with alcohol washes, then cleans 2-3 time by deionized water, standby after natural drying.
Embodiment 3
The present embodiment provides a kind of SERS substrate preparation method based on displacement method synthesis gold nano grain, described side
Method comprises the steps:
A: slide is sequentially placed into ultrasonic cleaning 5 minutes in acetone and alcohol, takes out after cleaning up by deionized water；
B: the vacuum of magnetron sputtering coater inner chamber is reached 10-5After Pa, zinc target power output is fixed on 50W, sets
Plated film time 100s；
C: start sputtering system, starts plated film；
D: the slide after the plated film of step c gained is put in the chlorauric acid solution that molar concentration is 0.05mmol/L, 35 DEG C
Lower immersion 20 minutes；
F: taken out by slide, first with alcohol washes, then cleans 2-3 time by deionized water, standby after natural drying.
Embodiment 4
The present embodiment provides a kind of SERS substrate preparation method based on reducing process synthesis gold nano grain, described side
Method comprises the steps:
A: slide is sequentially placed into ultrasonic cleaning 5 minutes in acetone and alcohol, takes out after cleaning up by deionized water；
B: the vacuum of magnetron sputtering coater inner chamber is reached 10-5After Pa, zinc target power output is fixed on 50W, sets
Plated film time 200s；
C: start sputtering system, starts plated film；
D: the slide after the plated film of step c gained is put in the chlorauric acid solution that molar concentration is 0.1mmol/L, 30 DEG C
Lower immersion 30 minutes；
F: taken out by slide, first with alcohol washes, then cleans 2-3 time by deionized water, standby after natural drying.
As shown in (a) in Fig. 1, the ESEM for SERS substrate surface gold nano grain in embodiment 1 shines
Sheet, as in Fig. 1, (b) show the transmission electron microscope photo of SERS substrate surface gold nano grain in example 2,
The visible SERS substrate surface gold nano grain not only distribution uniform prepared by method described in the present embodiment,
Grain is in the same size, and particle outline is clear, and mostly is torispherical particle.
As in figure 2 it is shown, be concentration 10-7The rhodamine (R6G) of mol/L is being made in embodiment 1,2,3 and 4
Standby suprabasil enhancing Raman spectrogram, it is seen that the SERS substrate prepared by method described in the present embodiment is to Luo Dan
Bright detectable limit reaches 10-7The order of magnitude, SERS strengthens respond well.
To sum up, the inventive method by vacuum magnetic-control sputtering technology at the zinc-plated film of surface of glass slide, then by it low dense
Degree (≤0.1mmol/L) chlorauric acid solution soaks, makes gold nano grain uniform by the method for zinc displacement gold chloride
The SERS substrate of high enhancer is made repeatably, had rhodamine to ground absorption, in slide substrate,.
Above the specific embodiment of the present invention is described.It is to be appreciated that the invention is not limited in
Stating particular implementation, those skilled in the art can make various deformation or amendment within the scope of the claims,
This has no effect on the flesh and blood of the present invention.
Claims (4)
1. a SERS substrate preparation method based on displacement method synthesis gold nano grain, it is characterised in that described
Method comprises the steps:
Step 1: slide is sequentially placed into ultrasonic cleaning in acetone and alcohol, takes out after cleaning up by deionized water；
Step 2: put in magnetron sputtering coater by the slide cleaned, forms zinc nano thin-film on slide；
Step 3: the slide after the plated film of step 2 gained is put into stirring reaction in chlorauric acid solution, is formed and adhere to table
The nano particle in face；
Step 4: the Wafer Cleaning that step 3 reacted also is dried, standby.
A kind of SERS substrate preparation side based on displacement method synthesis gold nano grain the most according to claim 1
Method, it is characterised in that in described step 2, including:
Step 2.1: the vacuum of magnetron sputtering coater inner chamber is reached 10-5～10-4After Pa, zinc target power output is fixed on
30～50W, set plated film time 20-200s；
Step 2.2: start sputtering system, starts plated film.
A kind of SERS substrate preparation side based on displacement method synthesis gold nano grain the most according to claim 1
Method, it is characterised in that in described step 3, including:
Step 3.1: the slide being coated with zinc film is put in the chlorauric acid solution that molar concentration is 0.01～0.1mmol/L,
Soak 5-30 minute at 30～35 DEG C；
Step 3.2: taken out by slide, first with alcohol washes, then cleans by deionized water, standby after natural drying.
4. according to a kind of based on displacement method synthesis gold nano grain the SERS base described in any one of claim 1-3
End preparation method, it is characterised in that in described step 4, cleans 2～3 by the slide substrate deionized water prepared
Secondary, natural drying final vacuum preserves, standby.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610261432.7A CN105755431A (en) | 2016-04-25 | 2016-04-25 | Preparation method for synthesizing gold nanoparticle-coated SERS substrate on basis of replacement method |
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| CN201610261432.7A CN105755431A (en) | 2016-04-25 | 2016-04-25 | Preparation method for synthesizing gold nanoparticle-coated SERS substrate on basis of replacement method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109570490A (en) * | 2018-12-28 | 2019-04-05 | 中国科学院合肥物质科学研究院 | The preparation method of the controllable hollow gold nano cap of sea urchin shape of extremely pure surface topography |
| CN115184339A (en) * | 2022-09-08 | 2022-10-14 | 海澳华(黑龙江)生物医药技术有限公司 | Method for rapidly detecting viruses based on portable Raman spectrometer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101566570A (en) * | 2009-05-27 | 2009-10-28 | 东南大学 | Orderly controllable surface-reinforced Raman scattering active substrate and preparation method thereof |
| CN102212790A (en) * | 2011-05-19 | 2011-10-12 | 浙江大学 | Preparation method of noble metal/submicron spherical shell arrays |
| CN105300956A (en) * | 2015-10-22 | 2016-02-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for Raman enhancement substrate |
-
2016
- 2016-04-25 CN CN201610261432.7A patent/CN105755431A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101566570A (en) * | 2009-05-27 | 2009-10-28 | 东南大学 | Orderly controllable surface-reinforced Raman scattering active substrate and preparation method thereof |
| CN102212790A (en) * | 2011-05-19 | 2011-10-12 | 浙江大学 | Preparation method of noble metal/submicron spherical shell arrays |
| CN105300956A (en) * | 2015-10-22 | 2016-02-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for Raman enhancement substrate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109570490A (en) * | 2018-12-28 | 2019-04-05 | 中国科学院合肥物质科学研究院 | The preparation method of the controllable hollow gold nano cap of sea urchin shape of extremely pure surface topography |
| CN109570490B (en) * | 2018-12-28 | 2021-01-22 | 中国科学院合肥物质科学研究院 | Preparation method of sea urchin-shaped hollow gold nanometer cap with controllable pure surface morphology |
| CN115184339A (en) * | 2022-09-08 | 2022-10-14 | 海澳华(黑龙江)生物医药技术有限公司 | Method for rapidly detecting viruses based on portable Raman spectrometer |
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