CN106404738A - Graphene oxide/silver nanoparticle/pyramid-shaped silicon three-dimensional Raman enhanced substrate and preparation method and application thereof - Google Patents
Graphene oxide/silver nanoparticle/pyramid-shaped silicon three-dimensional Raman enhanced substrate and preparation method and application thereof Download PDFInfo
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- CN106404738A CN106404738A CN201610802954.3A CN201610802954A CN106404738A CN 106404738 A CN106404738 A CN 106404738A CN 201610802954 A CN201610802954 A CN 201610802954A CN 106404738 A CN106404738 A CN 106404738A
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- graphene oxide
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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
Abstract
The invention provides a graphene oxide/silver nanoparticle/pyramid-shaped silicon three-dimensional Raman enhanced substrate and a preparation method and an application thereof. A pyramid-shaped silicon substrate is prepared by a wet etching process, the surface of the silicon substrate is coated with a silver nanoparticle solution, then the silver nanoparticle/pyramid-shaped silicon surface is coated with a graphene oxide solution, and baking treatment is performed. The preparation method has the advantages of simple operation, no toxicity, and no pollution, and eliminates tedious steps; moreover, the three-dimensional Raman enhanced substrate prepared by the method is combined with graphene oxide, silver nanoparticles and pyramid-shaped silicon, and can give full play to the advantages of the three components, to obtain a high-sensitivity, good-stability and high-homogeneity Raman enhanced signal; the key lies in that the graphene oxide/silver nanoparticle/pyramid-shaped silicon three-dimensional Raman enhanced substrate is prepared for the first time.
Description
Technical field
The invention belongs to Raman detection field, it is related to a kind of graphene oxide/silver nano-grain/pyramid silicon 3 D and draws
Graceful enhancing substrate and preparation method and application.
Background technology
Raman enhancement techniques as a kind of unmarked analysis detection meanss, due to its high sensitivity, in recent years
Cause the extensive concern of scientific research personnel.Scientific research personnel has done substantial amounts of work to obtain sensitivity height, good stability, equal
One stable Raman strengthens substrate.Research shows, for three-dimensional Raman enhancing substrate compares two dimension enhancing substrate, has larger
Specific surface area, thus the quantity of focus can be increased, it is especially advantageous for the absorption of testing molecule simultaneously, therefore can obtain highly sensitive
The Raman enhancing signal of degree.Three-dimensional Raman is strengthened substrate and is mainly obtained using photoetching process at present, and the method preparation process is more
Loaded down with trivial details, production cost is higher and inefficient, therefore limits its development.
Single metal strengthens base material although certain Raman reinforced effects can be obtained as Raman, but its
Electromagnetic enhancement effect is limited, sensitvity constraint, and metal surface is easily oxidized, and the stability of Raman enhancing signal is bad.
Content of the invention
The purpose of the present invention is exactly to solve the above problems, providing one kind to be based on graphene oxide/silver nano-grain/gold
Word turriform silicon 3 D Raman strengthens substrate and preparation method and application.The present invention is simple to operate, low cost, can achieve three-dimensional Raman
Strengthen the mass preparation of substrate, and the Raman enhancing signal sensitivity height obtaining, good stability, homogeneity are high.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of graphene oxide/silver nano-grain/pyramid silicon 3 D Raman strengthens substrate, described enhancing substrate under
Include pyramid silicon base, Silver nano-particle layer and graphene oxide layer to upper successively.
Three-dimensional pyramid silicon has periodic surface texture and larger specific surface area, can increase focus quantity,
Improve the enhanced sensitivity of Raman；Silver nano-grain compares for other metallic particles, and sensitivity is higher, and its surface is oxidizable
Unstability can be resolved by graphene oxide layer；And graphene oxide also has, and bio-compatibility is good, chemically stable
Property high advantage, the functional group that its surface exists is more easily implemented the special sex modification to its surface, thus realizing to biological point
The specific detection of son.
A kind of graphene oxide/silver nano-grain/pyramid silicon 3 D Raman strengthens the preparation method of substrate, including with
Lower step：
(1) base material is polished pretreatment, prepare pyramid silicon base；(2) coat silver to pyramid silicon base
Nanoparticles solution；(3) continue coating graphene oxide solution, baking, obtain final product.Achieve graphene oxide/Yin Na for the first time
Rice grain/pyramid silicon compound three-dimensional Raman strengthens the preparation of substrate.
Further, described silicon substrate material is monocrystal silicon.
Further, the method that described step (1) prepares pyramid silicon base is wet corrosion technique.
Further, described step (2) silver nanoparticle solution is the dispersion liquid of the homogeneous silver nano-grain of diameter.
Preferably, a diameter of 5-50nm of described silver nano-grain.
Further, in described step (3), the process of graphene oxide solution coating is dip-coating method at once.
The three-dimensional Raman of above-mentioned preparation strengthens application in obtaining Molecular Raman enhanced spectrum for the substrate.
Beneficial effects of the present invention：(1) present invention achieves based on graphene oxide/silver nano-grain/gold word first time
Turriform silicon 3 D Raman strengthens the preparation of substrate.
(2) preparation method of the present invention is simple to operate, eliminates loaded down with trivial details step, nontoxic pollution-free, can achieve three Wellas
The graceful mass preparation strengthening substrate.
(3) the pyramid silicon of the present invention has periodic surface texture, and specific surface area is larger, increased focus number
Amount, improves the enhanced sensitivity of Raman, and silica-base material reflectance is higher simultaneously, bio-compatibility is more preferable, surface is easy to cutting
And it is easy to functional modification；Be combined with Silver nano-particle layer using graphene oxide, on the one hand protect Silver nano-particle layer
Oxidation, on the other hand because graphene oxide bio-compatibility is good, chemical stability is high, is therefore especially advantageous for biomolecule
Absorption, and because the functional group that its surface exists makes graphene oxide be more easily implemented the special sex modification to its surface,
Thus can achieve the specific detection to biomolecule.
(4) graphene oxide/silver nano-grain that the present invention provides/pyramid silicon 3 D Raman strengthens substrate, effectively
The advantage combining graphene oxide, silver nano-grain and pyramid silicon three, the Raman enhancing signal sensitivity of acquisition
Height, good stability, homogeneity are high.
Brief description
Fig. 1 prepares, for the present invention, the signal that graphene oxide/silver nano-grain/pyramid silicon 3 D Raman strengthens substrate
Figure；
Fig. 2 prepares graphene oxide/silver nano-grain/pyramid silicon 3 D Raman for the embodiment of the present invention 1 and strengthens base
The scanning electron microscope image at bottom；
Fig. 3 is that the graphene oxide/silver nano-grain/pyramid silicon 3 D Raman of the embodiment of the present invention 1 preparation strengthens
Substrate obtains the Raman enhanced spectrum of R6G molecule；
Fig. 4 is that the graphene oxide/silver nano-grain/pyramid silicon 3 D Raman of the embodiment of the present invention 2 preparation strengthens
Substrate obtains the Raman enhanced spectrum of adenosine molecule.
Specific embodiment
The invention will be further described with embodiment below in conjunction with the accompanying drawings.Described material if no special instructions all can be from public affairs
Open commercial sources and obtain.
Embodiment 1
A kind of graphene oxide/silver nano-grain/pyramid silicon 3 D Raman strengthens substrate, described enhancing substrate under
Include pyramid silicon base, Silver nano-particle layer and graphene oxide layer to upper successively.Its preparation method includes following preparation
Step：
1. utilize wet corrosion technique to process monocrystalline silicon surface, prepared pyramid silicon base；
2., by silver nano-grain dispersion homogeneous for a diameter of 5nm to silicon substrate surface, obtain silver nano-grain/gold word
Turriform silicon face；
3. at once by graphene oxide dispersion dip-coating to silver nano-grain/pyramid silicon face；
4. baking is processed, that is, obtain graphene oxide/silver nano-grain/pyramid silicon 3 D Raman and strengthen substrate.
Embodiment 2
A kind of graphene oxide/silver nano-grain/pyramid silicon 3 D Raman strengthens substrate, described enhancing substrate under
Include pyramid silicon base, Silver nano-particle layer and graphene oxide layer to upper successively.Its preparation method includes following preparation
Step：
1. utilize wet corrosion technique to process monocrystalline silicon surface, prepared pyramid silicon base；
2., by silver nano-grain dispersion homogeneous for a diameter of 50nm to silicon substrate surface, obtain silver nano-grain/gold
Word turriform silicon face；
3. at once by graphene oxide dispersion dip-coating to silver nano-grain/pyramid silicon face；
4. baking is processed, that is, obtain graphene oxide/silver nano-grain/pyramid silicon 3 D Raman and strengthen substrate.
Prepare method schematic diagram such as Fig. 1 that graphene oxide/silver nano-grain/pyramid silicon 3 D Raman strengthens substrate
Shown.Graphene oxide/silver nano-grain that Fig. 2 is prepared for the embodiment of the present invention/pyramid silicon 3 D Raman strengthens substrate
Scanning electron microscope image, as can be seen from this figure：(1) the three-dimensional substrate that strengthens prepared has typical pyramid knot
Structure；(2) successfully achieve the compound of graphene oxide, silver nano-grain and pyramid silicon.
Embodiment 3
Graphene oxide/the silver nano-grain prepared by embodiment 1/pyramid silicon 3 D Raman is strengthened substrate be used for
Obtain the Raman enhanced spectrum of R6G molecule.
Fig. 3 prepares graphene oxide/silver nano-grain/pyramid silicon 3 D Raman for the present invention and strengthens substrate acquisition
The Raman enhanced spectrum of R6G molecule, as can be seen from this figure：Strengthen substrate using the three-dimensional Raman of preparation and obtain sensitivity
The Raman enhanced spectrum of the high R6G molecule of height, good stability, homogeneity.
Embodiment 4
Graphene oxide/the silver nano-grain prepared by embodiment 2/pyramid silicon 3 D Raman is strengthened substrate be used for
Obtain the Raman enhanced spectrum of adenosine molecule.
Fig. 4 prepares graphene oxide/silver nano-grain/pyramid silicon 3 D Raman for the present invention and strengthens substrate acquisition gland
The Raman enhanced spectrum of glycosides molecule, as can be seen from this figure：Using the three-dimensional Raman of preparation strengthen substrate obtain sensitivity height,
The Raman enhanced spectrum of the high adenosine molecule of good stability, homogeneity.
Although the above-mentioned accompanying drawing that combines is described to the specific embodiment of the present invention, not model is protected to the present invention
The restriction enclosed, one of ordinary skill in the art should be understood that on the basis of technical scheme, and those skilled in the art are not
Need to pay the various modifications that creative work can make or deformation still within protection scope of the present invention.
Claims (8)
1. a kind of graphene oxide/silver nano-grain/pyramid silicon 3 D Raman strengthens substrate, described enhancing substrate from lower to
On include pyramid silicon base, Silver nano-particle layer and graphene oxide layer successively.
2. a kind of graphene oxide/silver nano-grain/pyramid silicon 3 D Raman strengthens the preparation method of substrate, its feature
It is to comprise the following steps：
(1) base material is polished pretreatment, prepare pyramid silicon base；(2) coat silver nanoparticle to pyramid silicon base
Particle solution；(3) continue coating graphene oxide solution, baking, obtain final product.
3. a kind of graphene oxide/silver nano-grain/pyramid silicon 3 D Raman strengthens substrate as claimed in claim 2
Preparation method, is characterized in that, described silicon substrate material is monocrystal silicon.
4. a kind of graphene oxide/silver nano-grain/pyramid silicon 3 D Raman strengthens substrate as claimed in claim 2
Preparation method, is characterized in that, the method that described step (1) prepares pyramid silicon base is wet corrosion technique.
5. a kind of graphene oxide/silver nano-grain/pyramid silicon 3 D Raman strengthens substrate as claimed in claim 2
Preparation method, is characterized in that, described step (2) silver nanoparticle solution is the dispersion liquid of the homogeneous silver nano-grain of diameter.
6. a kind of graphene oxide/silver nano-grain/pyramid silicon 3 D Raman strengthens substrate as claimed in claim 5
Preparation method, is characterized in that, a diameter of 5-50nm of described silver nano-grain.
7. a kind of graphene oxide/silver nano-grain/pyramid silicon 3 D Raman strengthens substrate as claimed in claim 2
Preparation method, is characterized in that, in described step (3), the process of graphene oxide solution coating is dip-coating method at once.
8. graphene oxide/the silver nano-grain described in claim 1 or 2/pyramid silicon 3 D Raman strengthens substrate and is obtaining
Obtain the application in Molecular Raman enhanced spectrum.
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Cited By (7)
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| CN107189317A (en) * | 2017-05-17 | 2017-09-22 | 宁波大学 | A kind of silver/polymer/silver/graphene core-shell nano mushroom material and its preparation method and application |
| CN107462565A (en) * | 2017-07-21 | 2017-12-12 | 山东师范大学 | Silver-colored gyrus/graphene/golden film D S ERS substrates and preparation method |
| CN107860760A (en) * | 2017-11-09 | 2018-03-30 | 山东师范大学 | Graphene oxide/silver nano-grain/pyramid PMMA three-dimension flexibles Raman enhancing substrate and preparation method and application |
| CN108226137A (en) * | 2018-01-31 | 2018-06-29 | 山东师范大学 | A kind of flexible, transparent molybdenum disulfide@Argent grains/three-dimensional pyramid structure PMMA SERS substrates preparation method and application |
| CN108982471A (en) * | 2018-08-02 | 2018-12-11 | 江苏师范大学 | AgNR/O-g-C3N4Substrate, preparation method and its application in recyclable SERS Sensitive Detection |
| CN110819942A (en) * | 2019-11-13 | 2020-02-21 | 中国科学院合肥物质科学研究院 | Graphene oxide-coated nano-gold tube composite film and preparation method thereof |
| CN111504975A (en) * | 2020-06-04 | 2020-08-07 | 青岛峰峦新材料科技有限责任公司 | Transition metal disulfide enhanced graphene-based SERS device and preparation method thereof |
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Cited By (10)
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| CN107189317A (en) * | 2017-05-17 | 2017-09-22 | 宁波大学 | A kind of silver/polymer/silver/graphene core-shell nano mushroom material and its preparation method and application |
| CN107189317B (en) * | 2017-05-17 | 2019-06-18 | 宁波大学 | A kind of silver/polymer/silver/graphene core-shell nano mushroom material and its preparation method and application |
| CN107462565A (en) * | 2017-07-21 | 2017-12-12 | 山东师范大学 | Silver-colored gyrus/graphene/golden film D S ERS substrates and preparation method |
| CN107860760A (en) * | 2017-11-09 | 2018-03-30 | 山东师范大学 | Graphene oxide/silver nano-grain/pyramid PMMA three-dimension flexibles Raman enhancing substrate and preparation method and application |
| CN108226137A (en) * | 2018-01-31 | 2018-06-29 | 山东师范大学 | A kind of flexible, transparent molybdenum disulfide@Argent grains/three-dimensional pyramid structure PMMA SERS substrates preparation method and application |
| CN108982471A (en) * | 2018-08-02 | 2018-12-11 | 江苏师范大学 | AgNR/O-g-C3N4Substrate, preparation method and its application in recyclable SERS Sensitive Detection |
| CN108982471B (en) * | 2018-08-02 | 2021-01-08 | 江苏师范大学 | AgNR/O-g-C3N4Substrate, preparation method thereof and application thereof in recyclable SERS (surface enhanced Raman scattering) sensitive detection |
| CN110819942A (en) * | 2019-11-13 | 2020-02-21 | 中国科学院合肥物质科学研究院 | Graphene oxide-coated nano-gold tube composite film and preparation method thereof |
| CN111504975A (en) * | 2020-06-04 | 2020-08-07 | 青岛峰峦新材料科技有限责任公司 | Transition metal disulfide enhanced graphene-based SERS device and preparation method thereof |
| CN111504975B (en) * | 2020-06-04 | 2023-01-13 | 青岛峰峦新材料科技有限责任公司 | Transition metal disulfide enhanced graphene-based SERS device and preparation method thereof |
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