CN106967978A - Film of gold nano grain assembling and its production and use - Google Patents
Film of gold nano grain assembling and its production and use Download PDFInfo
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
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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
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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
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
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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
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/48—Electroplating: Baths therefor from solutions of gold
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/006—Nanoparticles
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- C25D7/00—Electroplating characterised by the article coated
- C25D7/12—Semiconductors
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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
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses film of a kind of gold nano grain assembling and its production and use.Film is to be covered with the film for mutually sticking into thick 2 μm of 200nm by multilayer gold nano grain in conductive substrates, wherein, the particle diameter of gold nano grain is 30 120nm, its gap or gap mutual for≤10nm；Method is the surface sputtering golden film prior to conductive substrates, obtains the conductive substrates that its surface is covered with golden film, then it is that negative electrode is placed in Gold electrolysis liquid that graphite flake is covered with into the conductive substrates of golden film as anode, its surface, and in electro-deposition under constant current, purpose product is made.It has higher SERS activity, be extremely easy to widely commercial applications in the quick trace detection to pesticide methyl parathion.
Description
Technical field
The present invention relates to a kind of film and preparation method and purposes, the film of especially a kind of gold nano grain assembling and its
Preparation method and purposes.
Background technology
Due to the resonance property of surface phasmon, noble metal nano structure or micro-nano structure are in Surface-enhanced spectroscopic, especially
In terms of SERS spectra, to have a wide range of applications.In the recent period, people are in order to your gold with surface plasmon resonance property obtained
Belong to micro-nano structure, made some good tries and effort, such as entitled " Facile Fabrication of High-Density
Sub-1-nm Gaps from Au Nanoparticle Monolayers as Reproducible SERS
Substrates ", Adv.Funct.Mater.2016,26, (" simplicity is prepared with high density sub- nano gap 8137-8145
Single layer of gold nano-particular film is used as repeatable SERS substrates ",《Advanced function material》, 8137-8145 of volume 26 in 2016
Page) article.The single layer of gold nano-particular film referred in this article is in being covered with silicon chip substrate by individual layer gold nano grain group
The film of dress；Preparation method is first obtains the single thin film that gold nano grain is assembled using liquid level self-assembly method, then by single thin layer
Film is transferred directly to clean silicon chip surface to obtain product.Though this product at 633nm and 785nm there is stronger light to inhale
Receive, weak point is but all there is with its preparation method, first, the gold nano grain in product is only individual layer, is not only constrained
Its SERS activity, its uniformity is also extremely easy to by the solution destruction to be measured such as water, so as to severely impact the equal of its SERS signal
Even property；Secondly, preparation method can not be obtained with higher SERS activity and by the solution to be measured such as water not destroyed its SERS signal equal
The product of even property.
The content of the invention
The technical problem to be solved in the present invention for overcome weak point of the prior art there is provided one kind it is rational in infrastructure,
SERS activity is higher, and is not destroyed the film of the gold nano grain assembling of its SERS signal uniformity by the solution to be measured such as water.
The invention solves the problems that another technical problem to provide a kind of preparation of the film of above-mentioned gold nano grain assembling
Method.
The invention solves the problems that another technical problem to provide a kind of purposes of the film of above-mentioned gold nano grain assembling.
To solve the technical problem of the present invention, the technical scheme used is the film of gold nano grain assembling includes lining
The film being made up of gold nano grain being covered with bottom, particularly：
The substrate is conductive substrates；
The film being made up of gold nano grain is that multilayer gold nano grain mutually sticks film forming, the multilayer gold nano
The thickness that particle mutually sticks the film of film forming is 200nm-2 μm；
The particle diameter of the gold nano grain is 30-120nm, its gap or gap mutual for≤10nm.
The further improvement of the film assembled as gold nano grain：
Preferably, conductive substrates are silicon chip substrate, or indium oxide tin glass substrate, or doping fluorine tin dioxide conductive glass
Glass substrate.
To solve another technical problem of the present invention, another technical scheme used is above-mentioned gold nano grain
It is as follows that the preparation method of the film of assembling includes sputtering method, particularly key step：
The golden film thick prior to the surface sputtering 10-30nm of conductive substrates, obtains the conductive substrates that its surface is covered with golden film, then
Graphite flake is covered with into the conductive substrates of golden film as anode, its surface to be placed in Gold electrolysis liquid for negative electrode, in 20-500 μ A/cm2
Constant current under electro-deposition 20-120min, be made gold nano grain assembling film.
The further improvement of the preparation method of the film assembled as gold nano grain：
Preferably, before golden film is sputtered to the surface of conductive substrates, ethanol and deionized water cleaning are first used for.
Preferably, after being cleaned 1-3 times using deionized water to the film that obtained gold nano grain is assembled, in 40-60 DEG C
Lower drying.
Preferably, conductive substrates are silicon chip substrate, or indium oxide tin glass substrate, or doping fluorine tin dioxide conductive glass
Glass substrate.
Preferably, Gold electrolysis liquid is 0.2-10g/L aqueous solution of chloraurate and 2-200g/L polyvinylpyrrolidone
(K30) mixed liquor of the aqueous solution.
Preferably, polyvinylpyrrolidone is the polyvinylpyrrolidone that its molecular weight is 40000.
To solve another technical problem of the present invention, another technical scheme used is above-mentioned gold nano grain
The purposes of the film of assembling is：
The film that gold nano grain is assembled uses the wavelength of exciting light as the active substrate of SERS
The content of the parathion-methyl adhered to thereon for 785nm laser Raman spectrometer measurement.
The further improvement of the purposes of the film assembled as gold nano grain：
Preferably, the power of the exciting light of laser Raman spectrometer be 0.1-2mW, the time of integration be 1-20s.
Beneficial effect relative to prior art is：
First, being characterized to obtained purpose product using ESEM, from its result, purpose product is substrate
On be covered with the film mutually sticked by multi-layer nano particle；Wherein, the thickness of film is 200nm-2 μm, the grain of nano particle
Footpath is 30-120nm, its gap or gap mutual for≤10nm.It is this that film group is mutually sticked into by multi-layer nano particle
The purpose product dressed up, both due to the surface plasmon resonance property that noble metal micro-nano structure possesses itself, and because of gold nano
Substantial amounts of gap or gap between particle and become induction SERS focus, SERS activity is drastically increased, due also to thin
Film is mutually sticked by multi-layer nano particle to be formed, and not only many times of ground improve its SERS activity, have also prevented water etc. to be measured molten
The uniformity of its SERS signal of the dissolved destruction of liquid, more because specific dimensions gold nano grain particle diameter and the thickness of film, and
It is to have stronger light absorbs at 785nm in exciting light to make it --- when using 785nm laser detection pesticide molecule, it can reduce sharp
Damage of the light to pesticide molecule, obtains the SERS spectra of molecule in itself, and can also reduce the interference of background signal, so that purpose
Product is provided with high SERS activity, is extremely suitable to the trace detection to pesticide molecule.
Second, using obtained purpose product as SERS active-substrate, through being carried out to parathion-methyl under various concentrations
The test of multiple many batches, when the concentration as little as 3 × 10 of measured object parathion-methyl–6During mol/L, remain to effectively detect it
Out, and its detection uniformity and repeatability in the multiple spot and any point in purpose product all very it is good.
Third, preparation method is simple, science, efficiently.Rational in infrastructure, SERS is not only made active higher, and not by water
Etc. the purpose product that solution to be measured destroys its SERS signal uniformity --- the film of gold nano grain assembling；Also make it have suitable
In the characteristic that trace detection is carried out to parathion-methyl, the characteristics of more having easy to operate quick；And then make purpose product easily
In widely commercial applications in the quick trace detection to pesticide methyl parathion.
Brief description of the drawings
Fig. 1 is one of result for being characterized to purpose product made from preparation method using ESEM (SEM).Its
In, a figures in Fig. 1 are the SEM image of purpose product, and b figures are the high magnification SEM image of purpose product shown in a figures；Fig. 1 is shown
Go out to constitute numerous gold nano grains of purpose product to there is substantial amounts of gap or gap between layered laminate, and particle.
Fig. 2 is that the purpose product for being attached with various concentrations parathion-methyl is characterized using laser Raman spectrometer
One of as a result.Curve I in Fig. 2 is containing 10–4The Raman light spectral line of the purpose product of mol/L parathion-methyls, curve II is containing 2
×10–5The Raman light spectral line of the purpose product of mol/L parathion-methyls, curve III is containing 3 × 10–6Mol/L parathion-methyls
The Raman light spectral line of purpose product.
Embodiment
The preferred embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Buy or be voluntarily made from market first：
It is used as the tin dioxide conductive glass lined of the silicon chip substrate of conductive substrates, indium oxide tin glass substrate and the fluorine that adulterates
Bottom；
Ethanol；
Deionized water.
Then：
Embodiment 1
What is prepared concretely comprises the following steps：
First cleaned using ethanol and deionized water after conductive substrates, in the thick golden films of the surface sputtering 10nm of conductive substrates；
Wherein, conductive substrates are indium oxide tin glass substrate, obtain the conductive substrates that its surface is covered with golden film.It regard graphite flake as sun again
Pole, its surface are covered with the conductive substrates of golden film and are placed in for negative electrode in Gold electrolysis liquid, in 20 μ A/cm2Constant current under electro-deposition
After 120min, be used for deionized water clean 1 time after, at 40 DEG C dry；Wherein, Gold electrolysis liquid is 0.2g/L gold chloride
The mixed liquor of the aqueous solution and 200g/L aqueous povidone solution, polyvinylpyrrolidone therein is that its molecular weight is
40000 polyvinylpyrrolidone, is made the film for being similar to the gold nano grain assembling shown in Fig. 1.
Embodiment 2
What is prepared concretely comprises the following steps：
First cleaned using ethanol and deionized water after conductive substrates, in the thick golden films of the surface sputtering 15nm of conductive substrates；
Wherein, conductive substrates are indium oxide tin glass substrate, obtain the conductive substrates that its surface is covered with golden film.It regard graphite flake as sun again
Pole, its surface are covered with the conductive substrates of golden film and are placed in for negative electrode in Gold electrolysis liquid, in 140 μ A/cm2Constant current under electro-deposition
After 95min, be used for deionized water clean 2 times after, at 45 DEG C dry；Wherein, Gold electrolysis liquid is 2.5g/L gold chloride
The mixed liquor of the aqueous solution and 150g/L aqueous povidone solution, polyvinylpyrrolidone therein is that its molecular weight is
40000 polyvinylpyrrolidone, is made the film for being similar to the gold nano grain assembling shown in Fig. 1.
Embodiment 3
What is prepared concretely comprises the following steps：
First cleaned using ethanol and deionized water after conductive substrates, in the thick golden films of the surface sputtering 20nm of conductive substrates；
Wherein, conductive substrates are indium oxide tin glass substrate, obtain the conductive substrates that its surface is covered with golden film.It regard graphite flake as sun again
Pole, its surface are covered with the conductive substrates of golden film and are placed in for negative electrode in Gold electrolysis liquid, in 260 μ A/cm2Constant current under electro-deposition
After 70min, be used for deionized water clean 2 times after, at 50 DEG C dry；Wherein, Gold electrolysis liquid is 5g/L gold chloride water
The mixed liquor of solution and 100g/L aqueous povidone solution, polyvinylpyrrolidone therein is that its molecular weight is
40000 polyvinylpyrrolidone, is made the film of gold nano grain assembling as shown in Figure 1.
Embodiment 4
What is prepared concretely comprises the following steps：
First cleaned using ethanol and deionized water after conductive substrates, in the thick golden films of the surface sputtering 25nm of conductive substrates；
Wherein, conductive substrates are indium oxide tin glass substrate, obtain the conductive substrates that its surface is covered with golden film.It regard graphite flake as sun again
Pole, its surface are covered with the conductive substrates of golden film and are placed in for negative electrode in Gold electrolysis liquid, in 380 μ A/cm2Constant current under electro-deposition
After 45min, be used for deionized water clean 3 times after, at 55 DEG C dry；Wherein, Gold electrolysis liquid is 7.5g/L gold chloride
The mixed liquor of the aqueous solution and 50g/L aqueous povidone solution, polyvinylpyrrolidone therein is that its molecular weight is
40000 polyvinylpyrrolidone, is made the film for being similar to the gold nano grain assembling shown in Fig. 1.
Embodiment 5
What is prepared concretely comprises the following steps：
First cleaned using ethanol and deionized water after conductive substrates, in the thick golden films of the surface sputtering 30nm of conductive substrates；
Wherein, conductive substrates are indium oxide tin glass substrate, obtain the conductive substrates that its surface is covered with golden film.It regard graphite flake as sun again
Pole, its surface are covered with the conductive substrates of golden film and are placed in for negative electrode in Gold electrolysis liquid, in 500 μ A/cm2Constant current under electro-deposition
After 20min, be used for deionized water clean 3 times after, at 60 DEG C dry；Wherein, Gold electrolysis liquid is 10g/L gold chloride water
The mixed liquor of solution and 2g/L aqueous povidone solution, polyvinylpyrrolidone therein is that its molecular weight is
40000 polyvinylpyrrolidone, is made the film for being similar to the gold nano grain assembling shown in Fig. 1.
Select respectively again in the silicon chip substrate as conductive substrates or the tin dioxide conductive glass substrate for the fluorine that adulterates, repetition
Embodiment 1-5 is stated, the film of the gold nano grain assembling shown in Fig. 1 has equally been made as or has been similar to.
The purposes of film of gold nano grain assembling is：
The film that gold nano grain is assembled uses the wavelength of exciting light as the active substrate of SERS
The content of the parathion-methyl adhered to thereon for 785nm laser Raman spectrometer measurement, obtains result as shown in Figure 2；Its
In, the power of the exciting light of laser Raman spectrometer be 0.1-2mW, the time of integration be 1-20s.
Obviously, those skilled in the art can to film and preparation method thereof of the gold nano grain assembling of the present invention and
Purposes carries out various changes and modification without departing from the spirit and scope of the present invention.So, if to these modifications of the invention
Belong to modification within the scope of the claims in the present invention and its equivalent technologies, then the present invention is also intended to comprising these changes and become
Including type.
Claims (10)
1. a kind of film of gold nano grain assembling, including the film being made up of gold nano grain being covered with substrate, its feature
It is：
The substrate is conductive substrates；
The film being made up of gold nano grain is that multilayer gold nano grain mutually sticks film forming, the multilayer gold nano grain
The thickness for mutually sticking the film of film forming is 200nm-2 μm；
The particle diameter of the gold nano grain is 30-120nm, its gap or gap mutual for≤10nm.
2. the film of gold nano grain assembling according to claim 1, it is characterized in that conductive substrates are silicon chip substrate, or oxygen
Change indium tin glass substrate, or doping fluorine tin dioxide conductive glass substrate.
3. the preparation method for the film that gold nano grain described in a kind of claim 1 is assembled, including sputtering method, it is characterised in that main
Want step as follows：
The golden film thick prior to the surface sputtering 10-30nm of conductive substrates, obtains the conductive substrates that its surface is covered with golden film, then by stone
Ink sheet is covered with the conductive substrates of golden film as anode, its surface and is placed in for negative electrode in Gold electrolysis liquid, in 20-500 μ A/cm2Perseverance
Determine electro-deposition 20-120min under electric current, the film of gold nano grain assembling is made.
4. the preparation method of the film of gold nano grain assembling according to claim 3, it is characterized in that to conductive substrates
Surface sputtering golden film before, be first used for ethanol and deionized water cleaning.
5. the preparation method of the film of gold nano grain assembling according to claim 3, it is characterized in that to obtained Jenner
After the film of rice grain assembling is cleaned 1-3 times using deionized water, in dry at 40-60 DEG C.
6. the preparation method of the film of gold nano grain assembling according to claim 3, it is characterized in that conductive substrates are silicon
Piece substrate, or indium oxide tin glass substrate, or doping fluorine tin dioxide conductive glass substrate.
7. the preparation method of the film of gold nano grain assembling according to claim 3, it is characterized in that Gold electrolysis liquid is
The mixed liquor of 0.2-10g/L aqueous solution of chloraurate and 2-200g/L aqueous povidone solution.
8. the preparation method of the film of gold nano grain assembling according to claim 7, it is characterized in that polyvinylpyrrolidine
Ketone is the polyvinylpyrrolidone that its molecular weight is 40000.
9. the purposes for the film that gold nano grain described in a kind of claim 1 is assembled, it is characterised in that：
The film that gold nano grain is assembled is using the wavelength of exciting light as the active substrate of SERS
The content for the parathion-methyl that 785nm laser Raman spectrometer measurement is adhered to thereon.
10. the purposes of the film of gold nano grain assembling according to claim 9, it is characterized in that laser Raman spectrometer
The power of exciting light be 0.1-2mW, the time of integration be 1-20s.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108982632A (en) * | 2018-07-26 | 2018-12-11 | 大连大学 | A kind of flexible electrode and preparation method thereof based on flower-like nanometer gold structure |
| CN109722683A (en) * | 2019-01-04 | 2019-05-07 | 中国科学院合肥物质科学研究院 | Gold nano structure and its preparation method and application with cone spiked surface |
| CN110487831A (en) * | 2019-07-30 | 2019-11-22 | 西南交通大学 | The preparation method of speckle and the method and apparatus for preparing nanogold particle coating speckle |
| CN110579461A (en) * | 2019-05-15 | 2019-12-17 | 上海交通大学 | Preparation method and application of SERS performance detection biosensor |
| NL2028411A (en) * | 2020-06-10 | 2021-08-30 | Qingdao Univ Of Science And Technology | RAMAN-ENHANCED SUBSTRATE, FABRICATION METHOD THEREOF, AND METHOD FOR DETECTING miRNA |
| CN113668029A (en) * | 2021-08-27 | 2021-11-19 | 安徽大学 | Film formed by rough gold nanoparticles and preparation method and application thereof |
| CN114672858A (en) * | 2022-04-27 | 2022-06-28 | 安徽大学 | Nano gold film for enhancing Raman scattering activity and preparation method thereof |
Citations (2)
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| CN105174194A (en) * | 2015-08-06 | 2015-12-23 | 中国科学院合肥物质科学研究院 | Gold micro-nano structure array and preparation method as well as application thereof |
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| CN102944545A (en) * | 2012-12-05 | 2013-02-27 | 江西师范大学 | Layered three-dimensional structure nanogold surface enhanced Raman active substrate and preparation method thereof |
| CN105174194A (en) * | 2015-08-06 | 2015-12-23 | 中国科学院合肥物质科学研究院 | Gold micro-nano structure array and preparation method as well as application thereof |
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| CN108982632A (en) * | 2018-07-26 | 2018-12-11 | 大连大学 | A kind of flexible electrode and preparation method thereof based on flower-like nanometer gold structure |
| CN109722683A (en) * | 2019-01-04 | 2019-05-07 | 中国科学院合肥物质科学研究院 | Gold nano structure and its preparation method and application with cone spiked surface |
| CN110579461A (en) * | 2019-05-15 | 2019-12-17 | 上海交通大学 | Preparation method and application of SERS performance detection biosensor |
| CN110487831A (en) * | 2019-07-30 | 2019-11-22 | 西南交通大学 | The preparation method of speckle and the method and apparatus for preparing nanogold particle coating speckle |
| CN110487831B (en) * | 2019-07-30 | 2022-01-07 | 西南交通大学 | Preparation method of speckles and method and equipment for preparing gold nanoparticle coating speckles |
| NL2028411A (en) * | 2020-06-10 | 2021-08-30 | Qingdao Univ Of Science And Technology | RAMAN-ENHANCED SUBSTRATE, FABRICATION METHOD THEREOF, AND METHOD FOR DETECTING miRNA |
| CN113668029A (en) * | 2021-08-27 | 2021-11-19 | 安徽大学 | Film formed by rough gold nanoparticles and preparation method and application thereof |
| CN113668029B (en) * | 2021-08-27 | 2023-03-10 | 安徽大学 | Film formed by rough gold nanoparticles and preparation method and application thereof |
| CN114672858A (en) * | 2022-04-27 | 2022-06-28 | 安徽大学 | Nano gold film for enhancing Raman scattering activity and preparation method thereof |
| CN114672858B (en) * | 2022-04-27 | 2023-09-19 | 安徽大学 | Nano gold film for enhancing Raman scattering activity and preparation method thereof |
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