CN104730059B - A kind of lattice array surface enhanced Raman substrate and preparation method - Google Patents
A kind of lattice array surface enhanced Raman substrate and preparation method Download PDFInfo
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Abstract
The present invention relates to a kind of surface enhanced Raman substrate technology, more particularly to a kind of lattice array surface enhanced Raman substrate and preparation method.Preparation method comprises the following steps successively：A, the iron oxide particle for preparing uniform particle sizes；B, in iron oxide particle outer cladding layer gold, obtain magnetic nanoparticle covered with gold leaf；C, the silicon chip substrate for preparing the pit that declined with lattice array；Dried up after d, silicon chip substrate cleaning；E, by the silicon chip substrate hydrophilic treated；F, under the sucking action of magnet, by magnetic nanoparticle covered with gold leaf be enriched in nick hole in；The excessive magnetic nanoparticle covered with gold leaf cheated in nick on g, cleaning silicon wafer substrate, obtains hard surface enhancing Raman substrate.The lattice array surface enhanced Raman substrate of the present invention, is made by preceding method.The lattice array surface enhanced Raman substrate preparation method of the present invention, can prepare the active substrate that sensitivity is higher, repeated preferable, stable homogeneous is higher.
Description
Technical field
The present invention relates to a kind of surface enhanced Raman substrate technology, more particularly to a kind of lattice array surface enhanced Raman substrate
And preparation method.
Background technology
SERS (Surface-enhanced Raman Scattering, SERS) was sent out from 1974
Since existing, just cause everybody and widely paid close attention to, because it has very high sensitivity, be able to detect that absorption in metal surface
The molecule of monolayer and sub- monolayer, can provide the structural information of surface molecular again, it is considered to be a kind of very effective
Detect interfacial characteristics and intermolecular interaction, the instrument for characterizing surface molecular adsorption behavior and molecular structure.SERS technologies by
Gradually turn into Surface Science and the strong research meanses of electrochemical field, and trace analysis or even Single Molecule Detection, chemistry and
It is widely applied in research in terms of industry, environmental science, biomedical system, nano material and sensor, very
To the combination for occurring in that Raman technology and other technologies.
In view of SERS technologies have a wide range of applications, prepare that a kind of stability is high, enhancing effect is good, reappearance is strong
SERS active-substrate turns into key component.Conventional traditional SERS active-substrate is many at present, such as：Your Electrochemical roughening gold
Belong to active electrode substrate, noble metal colloidal sol active substrate, vacuum evaporation noble metal island film activity substrate and chemical etching and change
The active substrate of depositing noble metal is learned, but the surface roughness that these self-assembly activity substrates are provided is difficult to control to, thus shadow
The stability, homogeneity and repeatability of binding molecule spectrum are rung.Recent study it is more prepare orderly surface nano-structure
Method have some prepare and apply upper shortcomings and limitations, for example：With prepared by beamwriter lithography and scanning sonde method
Surface nano-structure area very little, low yield, equipment is expensive；For self-organizing growth method and nano-imprint method, generally compared with
The structural parameters of hardly possible regulation surface nano-structure.And because its preparation procedure is cumbersome, prepares cost height and preparation efficiency is low
Its development is limited etc. reason.Therefore urgent need exploitation is a kind of efficient, flexible, inexpensive, can prepare high sensitivity, repeatable, homogeneous
The surface enhanced Raman substrate preparation method of stable surface nano-structure.
The content of the invention
In order to solve the above technical problems, it is an object of the invention to provide one kind can prepare sensitivity it is higher, it is repeated compared with
The lattice array surface enhanced Raman substrate preparation method of the higher active substrate of good, stable homogeneous.
The present invention provides a kind of lattice array surface enhanced Raman substrate preparation method, comprises the following steps successively：
A, prepare the iron content of uniform particle sizes, cobalt or nickel metal oxide magnetic nanoparticle, due to iron, cobalt, nickel three
Kind of ferromagnetic element is the basic constituent element for constituting magnetic material, and magnetic property has a high similarity, and ferrous metal oxide
Production cost it is relatively low, the present invention be only described further with iron oxide particle；
B, in magnetic nanoparticle outer cladding layer gold, obtain magnetic nanoparticle covered with gold leaf；Wherein, gold is to be used to strengthen Raman
Material, gold be elemental gold, be gold crystal；
C, the silicon chip substrate for preparing the pit that declined with lattice array；
Dried up after d, silicon chip substrate cleaning；
E, by the silicon chip substrate hydrophilic treated；
F, under the sucking action of magnet, by magnetic nanoparticle covered with gold leaf be enriched in nick hole in；
The excessive magnetic nanoparticle covered with gold leaf cheated in nick on g, cleaning silicon wafer substrate, obtains hard surface enhancing Raman base
Bottom.
Specifically, in the step a, the magnetic nanoparticle is iron oxide particle.
Specifically, in the step a, the magnetic nanoparticle of uniform particle sizes is prepared by hydro-thermal method.
Specifically, in the step b, by situ synthesis in magnetic nanoparticle outer cladding layer gold.
Specifically, in the step c, the silicon chip substrate with micro- pit array is prepared with photoetching process.
Specifically, in the step d, after silicon chip substrate is cleaned by ultrasonic successively using acetone, ethanol and deionized water, using
Nitrogen gun is dried up.
Specifically, in the step e, the silicon chip substrate, which is put into do in plasma washing machine, is not less than the hydrophilic of 1min
Processing.
Further, step h and step i are also carried out after the step a-g, wherein,
H, by before solidification hydrogel filling be covered in hard surface enhancing Raman substrate on；
I, after after water-setting adhesive curing, it is peeled off from silicon chip substrate, obtain soft surface enhancing Raman substrate.
The present invention also provides a kind of lattice array surface enhanced Raman substrate, including hard surface enhancing Raman substrate and
Soft surface strengthens two kinds of forms of Raman substrate, wherein, the hard surface enhancing Raman substrate includes silicon chip substrate and gold filled
It is provided with lattice array in magnetic nanoparticle, the silicon chip substrate to decline pit, the magnetic nanoparticle covered with gold leaf is enriched in institute
State in nick hole；The soft surface enhancing Raman substrate includes hydrogel substrate and magnetic nanoparticle covered with gold leaf, the water-setting
It is provided with matrix bottom in dot matrix column projection, the projection and is embedded with the magnetic nanoparticle covered with gold leaf；The magnetic covered with gold leaf
Nano particle is the magnetic nanoparticle for being coated with layer gold, and the magnetic nanoparticle is iron oxide particle.
By such scheme, the present invention at least has advantages below：Magnetic nanoparticle is prepared by hydro-thermal method, then
Magnetic nanoparticles covered with gold leaf regular, with uniform particle sizes are prepared by situ synthesis, and by micro- in silicon template
Pit border physical constraint and magnetic nanoparticle covered with gold leaf is regulated and controled by magnetic closely arranged assembling, significantly improve unit bodies
The mode of SERS hotspot densities in product, to increase the sensitivity, repeatability and homogeneity of SERS detection signals.What this invention was obtained
Surface enhanced Raman substrate, it is practical, the characteristics of repeated with magnetite gathering boundary constraint, lattice array, so that there is provided one
Plant new sensitive SERS detections substrate.This invention can also by magnetite gathering, regulate and control iron oxide nanoparticles between away from
From thus obtaining the different-effect for surface-enhanced Raman.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, below with presently preferred embodiments of the present invention and coordinate accompanying drawing describe in detail as after.
Brief description of the drawings
Fig. 1 is the flow chart of the lattice array surface enhanced Raman substrate preparation method of the present invention；
Fig. 2 is the shape appearance figure of the transmission electron microscope of magnetic nanoparticle covered with gold leaf in the embodiment of the present invention one；
Fig. 3 is the shape appearance figure of the SEM of magnetic nanoparticle covered with gold leaf in the embodiment of the present invention one；
Fig. 4 be the embodiment of the present invention one in sprawl nanometer in the micro- pit array of silicon chip substrate with the method for magnetite gathering
The shape appearance figure of SEM after grain；
Fig. 5 is that soft surface strengthens shape appearance figure of the Raman substrate under the conditions of light microscope bright field illumination；
Fig. 6 strengthens the Raman spectrum result of Raman substrate for rhodamine R6G in the embodiment of the present invention two using hard surface
Comparison diagram；
Fig. 7 strengthens the Raman spectrum result of Raman substrate for rhodamine R6G in the embodiment of the present invention two using soft surface
Comparison diagram.
Embodiment
With reference to the accompanying drawings and examples, the embodiment to the present invention is described in further detail.Implement below
Example is used to illustrate the present invention, but is not limited to the scope of the present invention.
Embodiment one
The present invention provides a kind of lattice array surface enhanced Raman substrate preparation method, as shown in figure 1, including following step successively
Suddenly：
A, the iron oxide particle by hydro-thermal method preparation uniform particle sizes.
Hydro-thermal method refers to that in sealed pressure vessel water is solvent, and the chemistry carried out under conditions of HTHP is anti-
Should.Hydro-thermal method is to make those insoluble or indissoluble material dissolvings, or instead in atmospheric conditions using the aqueous solution of HTHP
The lysate of the material should be generated, by controlling the temperature difference of solution in autoclave to make generation convection current to form hypersaturated state and
The method for separating out growth crystal.Specifically preparation method is：1.08g Iron(III) chloride hexahydrates, 4g anhydrous sodium acetates are in vigorous magnetic
Under stirring, in the mixed solution for adding 14mL ethylene glycol and 26mL diethylene glycols, solid dissolving, obtained khaki solution.Will
This solution mean allocation is transferred in the steel bomb of three 20mL polytetrafluoroethylene (PTFE), is sealed and is heated to 200 in baking oven
℃.After reaction 15 hours, reactor is placed in room temperature and cooled down.The ferroso-ferric oxide obtained twice is cleaned with water and ethanol respectively
Nano particle, is dried in vacuo 12 hours.
In addition to hydro-thermal method, ferriferrous oxide particles can be also prepared using sol-gel process, the method is to use Fe3+, second
Alcohol, ethylene glycol are configured to colloidal sol, and ferriferrous oxide film is made using the autoreduction ability of system at 300-1000 DEG C, but
The ferriferrous oxide particles effect that this method is prepared is not good, and particle is presented spherical on product film, and has a large amount of crystal to lack
Fall into, particle size is because heat treatment condition is different and is between 40-188nm.
B, by situ synthesis in iron oxide particle outer cladding layer gold.
In situ synthesis refers to that the method is simple, controllable, and can fast make in material surface direct growth next step material
Obtain uniform core shell structure.It can also access functional group by surface modification to connect in the method for magnetic nanoparticle outer layer covers gold
Gold grain is connect, but particle is unstable made from the method, easily produces functional group and comes off, connects unstable shortcoming.Pass through
In situ synthesis consolidates difficult for drop-off and uniform particle sizes in iron oxide particle outer cladding layer gold, obtained layer gold.Specific experiment
Process is as follows：
20mg is dissolved in 5mL tetrahydrofurans, under conditions of ultrasound, and the 2mL water dissolved with 20mg dopamine hydrochlorides is delayed
It is slow to instill in tetrahydrofuran, ultrasound one hour.Mixed liquor is put into be stirred overnight at room temperature.The side of excessive dopamine Magneto separate
Formula is removed.Obtained ferroso-ferric oxide-dopamine particle is scattered in 20mL water.
It is prepared by golden kind：Classics prepare experiment, and 12 μ L 80%THPC and 250 μ L NaOH (2M) are added sequentially to going for 45mL
In ionized water.It is stirred vigorously after five minutes, 2mL 1% gold chloride is added into above-mentioned solution, and lucifuge is stirred overnight.
Golden growth-promoting media：The gold chlorides of 1.5mL 1% are added in the 100mL deionized waters dissolved with 25mg potassium carbonate.10 minutes
Afterwards, solution becomes colourless.Growth-promoting media stands overnight standby.
Gold plants absorption：The negatively charged gold in surface is planted can be adsorbed in four amine-modified oxidations of DOPA by electrostatic interaction
The surface of three iron particles.8mL gold plants dopamine-ferroso-ferric oxide (1mg/mL that solution is added to 5mL–1) in suspension.
0.2M acetic acid is instilled in this growth-promoting media, and pH value of solution is adjusted into 4 or so.Mixed liquor acutely rocks overnight.Magneto separate and clean
Excessive gold is planted and removed by mode.
Layer gold grows：In order to form the golden shell of thick-layer, the method for this growth in situ is used.100mL golden growth-promoting media is in play
Dopamine-ferriferrous oxide particles solution (1mg/mL that 5mL has adsorbed golden kind is added under conditions of strong stirring–1) in, with 29%
Formalin as reducing agent, be added dropwise in above-mentioned solution, until solution become dusty blue.
By in situ synthesis in iron oxide particle outer cladding layer gold, as shown in Figures 2 and 3 shaggy is made
Magnetic nanoparticle covered with gold leaf, wherein Fig. 2 are the transmission electron microscope photo of magnetic nanoparticle covered with gold leaf, illustrate surface parcel
Nano particle pattern after coarse layer gold, Fig. 3 is the electron scanning micrograph of gold-covered nano particle, from Fig. 2 and Fig. 3
As can be seen that preparing having good uniformity for nano particle, particle diameter is in 138 rans.
C, the silicon chip substrate with micro- pit array is prepared with photoetching process.
Photoetching process is to utilize photoimaging and the light-sensitive emulsion patterned process in substrate such as silicon material.Photoetching process is due to it
The advantage that design is accurate, error is small, applied widely, reproducible, the process for designing and producing template.Experimental method is such as
Under：Base is used as using 4 inches of the crystal face silicon chips of n-type 100 (LuoYang Single Crystal Silicon Co.China)
Piece.Then one layer 300 nanometers of ultra-thin aluminium lamination is being sputtered thereon.Again with the technology of ultraviolet photolithographic by mask plate by aluminium surface
2 microns of thick photoresists (RZJ304) pattern is made.Unnecessary photoresist is removed with nitric acid, potassium hydroxide solution pair is used
Aluminium lamination is performed etching.Using etched aluminium lamination as template, silicon layer is etched using inductively coupled plasma, you can finally prepare
The microarray template of suitable dimension.
After d, silicon chip substrate are cleaned by ultrasonic successively using acetone, ethanol and deionized water, dried up using nitrogen gun.
E, silicon chip substrate, which are put into, does the hydrophilic treated for being not less than 1min in plasma washing machine.
F, as seen in figs. 1 a-1b, under the sucking action of magnet, magnetic nanoparticle covered with gold leaf is enriched in nick hole；
G, as shown in Figure 1 C, the excessive magnetic nanoparticle covered with gold leaf cheated in nick, is obtained such as Fig. 4 institutes in cleaning silicon wafer substrate
Magnetic covered with gold leaf is uniformly paved with nick hole in the hard surface enhancing Raman substrate shown, Fig. 4 hard surfaces enhancing Raman substrate
Nano particle, and smooth and clean outside pit, as shown in figure iD, hard surface enhancing Raman substrate can be under laser to it
Its material does Raman detection.
H, as referring to figure 1E, the hydrogel filling before solidification is covered in hard surface enhancing Raman substrate；
I, as shown in fig. 1F, after after water-setting adhesive curing, it is peeled off from silicon chip substrate, obtains as shown in Figure 5 soft
Deeper face is presented to displaced the gel micro-protuberance of gold-covered nano granular materials thereon in surface enhanced Raman substrate, circle
Color, blank parts are then the smooth pattern-free part of gel.
Wherein, lattice array surface enhanced Raman substrate of the invention, including hard surface strengthen Raman substrate and soft
Two kinds of forms of surface enhanced Raman substrate, wherein, hard surface enhancing Raman substrate includes silicon chip substrate and magnetic Nano covered with gold leaf
It is provided with lattice array in particle, silicon chip substrate to decline pit, magnetic nanoparticle covered with gold leaf is enriched in nick hole, and hard surface increases
Strong Raman substrate is made up of above-mentioned steps a-g；Soft surface enhancing Raman substrate includes hydrogel substrate and magnetic Nano covered with gold leaf
It is provided with particle, hydrogel substrate in dot matrix column projection, projection and is embedded with magnetic nanoparticle covered with gold leaf, soft surface enhancing
Raman substrate is made up of above-mentioned steps a-i；Magnetic nanoparticle covered with gold leaf is the iron oxide particle for being coated with layer gold.
Embodiment two
The present invention provides the lattice array surface enhanced Raman substrate in embodiment one, to the rhodamine 6G (10 of various concentrations- 5M、10-6M、10-7M Raman detection result) is done.
As shown in Figure 6 and Figure 7, respectively hard and soft surface enhanced Raman substrate to various concentrations R6G detect
As a result displaying contrast；As shown in fig. 6, the boundary constraint lattice array for the hard prepared as surface Raman enhancement substrate to not
Same concentration (10-5、10-6、10-7M R6G solution) has very strong Raman signal, its Raman spectrum feature peak position 1180,
1313rd, 1363,1510,1575 and 1650cm-1Intensity be also high-visible, R6G solid refer to R6G solids in figure,
Concentration is considered as 1M, and test limit (LOD) is about 10-7M.As shown in fig. 7, the soft boundary constraint lattice array prepared is made
It is surface Raman enhancement substrate to various concentrations (10-4、10-5) R6G solution have stronger Raman signal, its Raman spectrum exists
Feature peak position 1180,1313,1363,1510,1575 and 1650cm-1Intensity be also high-visible.R6G solid refer in figure
Be R6G solids, concentration is considered as 1M, and test limit (LOD) is about 10-5M.It is soft to strengthen Raman substrate phase with hard surface
Than its test limit (LOD) is higher.
Described above is only the preferred embodiment of the present invention, is not intended to limit the invention, it is noted that for this skill
For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is some improvement and
Modification, these improvement and modification also should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of lattice array surface enhanced Raman substrate preparation method, it is characterised in that：Comprise the following steps successively：
A, prepare the iron content of uniform particle sizes, cobalt or nickel metal oxide magnetic nanoparticle；
B, in magnetic nanoparticle outer cladding layer gold, obtain magnetic nanoparticle covered with gold leaf；
C, the silicon chip substrate for preparing the pit that declined with lattice array；
Dried up after d, silicon chip substrate cleaning；
E, by the silicon chip substrate hydrophilic treated；
F, under the sucking action of magnet, by magnetic nanoparticle covered with gold leaf be enriched in nick hole in；
The excessive magnetic nanoparticle covered with gold leaf cheated in nick on g, cleaning silicon wafer substrate, obtains hard surface enhancing Raman substrate,
H, by before solidification hydrogel filling be covered in hard surface enhancing Raman substrate on；
I, after after water-setting adhesive curing, it is peeled off from silicon chip substrate, obtain soft surface enhancing Raman substrate.
2. lattice array surface enhanced Raman substrate preparation method according to claim 1, it is characterised in that：The step a
In, the magnetic nanoparticle is iron oxide particle.
3. lattice array surface enhanced Raman substrate preparation method according to claim 1, it is characterised in that：The step a
In, the magnetic nanoparticle of uniform particle sizes is prepared by hydro-thermal method.
4. lattice array surface enhanced Raman substrate preparation method according to claim 1, it is characterised in that：The step b
In, by situ synthesis in magnetic nanoparticle outer cladding layer gold.
5. lattice array surface enhanced Raman substrate preparation method according to claim 1, it is characterised in that：The step c
In, the silicon chip substrate with micro- pit array is prepared with photoetching process.
6. lattice array surface enhanced Raman substrate preparation method according to claim 1, it is characterised in that：The step d
In, after silicon chip substrate is cleaned by ultrasonic successively using acetone, ethanol and deionized water, dried up using nitrogen gun.
7. lattice array surface enhanced Raman substrate preparation method according to claim 1, it is characterised in that：The step e
In, the silicon chip substrate, which is put into, does the hydrophilic treated for being not less than 1min in plasma washing machine.
8. a kind of lattice array surface enhanced Raman substrate, it is characterised in that：Strengthen Raman substrate and soft including hard surface
Two kinds of forms of surface enhanced Raman substrate, wherein, the hard surface enhancing Raman substrate includes silicon chip substrate and magnetic covered with gold leaf
It is provided with lattice array in nano particle, the silicon chip substrate to decline pit, the magnetic nanoparticle covered with gold leaf is enriched in described micro-
In pit；The soft surface enhancing Raman substrate includes hydrogel substrate and magnetic nanoparticle covered with gold leaf, the water-setting matrix
It is provided with bottom in dot matrix column projection, the projection and is embedded with the magnetic nanoparticle covered with gold leaf, the magnetic Nano covered with gold leaf
Particle is the magnetic nanoparticle for being coated with layer gold.
9. lattice array surface enhanced Raman substrate according to claim 8, it is characterised in that：The magnetic nanoparticle is
Iron oxide particle.
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| CN104237202B (en) * | 2014-09-18 | 2017-03-15 | 苏州大学 | A kind of silicon nano-array substrate and preparation method thereof, application |
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| CN110044872A (en) * | 2019-05-10 | 2019-07-23 | 山东大学 | A kind of surface enhanced Raman substrate and the preparation method and application thereof |
| CN110044872B (en) * | 2019-05-10 | 2021-02-12 | 山东大学 | Surface-enhanced Raman substrate and preparation method and application thereof |
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