CN104730059A - Point-array surface enhanced raman substrate and preparation method - Google Patents
Point-array surface enhanced raman substrate and preparation method Download PDFInfo
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Abstract
The invention relates to the technology of the surface enhanced raman substrate, and particularly relates to a point-array surface enhanced raman substrate and a preparation method. The preparation method comprises the following steps: a. preparing iron oxide particles with uniform particle size; b. covering each iron oxide particle with a gold layer to obtain a gold-cladding magnetic nano particle; c. preparing a silicon chip substrate with point-array micro pits; d. washing the silicon chip substrate, and drying the silicon chip substrate; e. carrying out hydrophilic treatment on the silicon chip substrate; f. gathering the gold-cladding magnetic nano particles in the micro pits; and g. cleaning the gold-cladding magnetic nano particles overflowing from the micro pits on the silicon chip substrate to obtain the hard surface enhanced raman substrate. The point-array surface enhanced raman substrate is prepared in the method. By adopting the preparation method, the active substrate with high sensitivity, good repetition and high uniformity and stability can be prepared.
Description
Technical field
The present invention relates to a kind of surface enhanced Raman substrate technology, particularly relate to a kind of lattice array surface enhanced Raman substrate and preparation method.
Background technology
Surface enhanced raman spectroscopy (Surface-enhanced Raman Scattering, SERS) since being found from 1974, just cause everybody to pay close attention to widely, because it has very high sensitivity, the molecule of unimolecular layer and the sub-unimolecular layer being adsorbed on metal surface can be detected, the structural information of surface molecular can be provided again, be considered to the instrument of a kind of very effective detection interfacial characteristics and intermolecular interaction, characterizing surface molecular absorption behavior and molecular structure.SERS technology becomes Surface Science and the strong research means of electrochemical field gradually, and in trace analysis and even Single Molecule Detection, chemistry and industry, environmental science, biomedical system, be widely applied in the research of nano material and sensor aspect, even occurred the coupling of Raman technology and other technologies.
In view of SERS technology has a wide range of applications, prepare a kind of stability high, strengthen effective, that reappearance is strong SERS active-substrate and become key component.Traditional SERS active-substrate conventional is at present a lot, as: Electrochemical roughening noble metal active electrode basement, noble metal colloidal sol active substrate, the active substrate of the film activity substrate of vacuum evaporation noble metal island and chemical etching and chemogenic deposit noble metal, but the surfaceness that these self assembly active substrates provide is difficult to control, and thus have impact on the stability of binding molecule spectrum, homogeneity and repeatability.The method of the orderly surface nano-structure of preparation that Recent study is more has the shortcomings and limitations on some Synthesis and applications, such as: very little with the area of beamwriter lithography and the surface nano-structure prepared by scan-probe method, productive rate is low, apparatus expensive; For self-organizing growth method and nano-imprint method, the structural parameters of more difficult adjustment surface nano-structure usually.And due to its preparation procedure loaded down with trivial details, the reasons such as the high and preparation efficiency of preparation cost is low limit its development.Therefore be badly in need of exploitation a kind of efficient, flexibly, low cost, high sensitivity can be prepared, can repeat, the surface enhanced Raman substrate preparation method of the surface nano-structure of stable homogeneous.
Summary of the invention
For solving the problems of the technologies described above, the object of this invention is to provide a kind of lattice array surface enhanced Raman substrate preparation method that can prepare the active substrate that sensitivity is higher, repeatability is better, stable homogeneous is higher.
The invention provides a kind of lattice array surface enhanced Raman substrate preparation method, comprise the following steps successively:
The magnetic nanoparticle of the metal oxide of a, the iron content preparing uniform particle sizes, cobalt or nickel, because iron, cobalt, nickel three kinds of ferromagnetic elements are the basic constituent elements forming magnetic material, and magnetic property has high similarity, and the production cost of ferrous metal oxide is lower, the present invention is 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 the material for strengthening Raman, and gold is elemental gold, is the crystal of gold;
C, prepare have lattice array decline pit silicon wafer-based at the bottom of;
Dry up after cleaning at the bottom of d, described silicon wafer-based;
E, by hydrophilic treatment at the bottom of described silicon wafer-based;
F, under the sucking action of magnet, magnetic nanoparticle covered with gold leaf is enriched in nick hole in;
Excessive in the magnetic nanoparticle covered with gold leaf in nick hole in g, cleaning silicon wafer substrate, obtain hard surface and strengthen Raman substrate.
Concrete, in described step a, described magnetic nanoparticle is iron oxide particle.
Concrete, in described step a, prepared the magnetic nanoparticle of uniform particle sizes by hydro-thermal method.
Concrete, in described step b, by situ synthesis in magnetic nanoparticle outer cladding layer gold.
Concrete, in described step c, prepare at the bottom of the silicon wafer-based with micro-pit array by photoetching process.
Concrete, in described steps d, adopt acetone, ethanol and deionized water at the bottom of silicon wafer-based successively after ultrasonic cleaning, use nitrogen gun to dry up.
Concrete, in described step e, at the bottom of described silicon wafer-based, put into the hydrophilic treatment that plasma washing machine is not less than 1min.
Further, after described step a-g, also carry out step h and step I, wherein,
H, the hydrogel before solidification filled cover hard surface and strengthen in Raman substrate;
I, until hydrogel solidification after, it is peeled off at the bottom of silicon wafer-based, obtain soft surface strengthen Raman substrate.
The present invention also provides a kind of lattice array surface enhanced Raman substrate, comprise hard surface and strengthen Raman substrate and soft surface enhancing Raman substrate two kinds of forms, wherein, described hard surface strengthens Raman substrate and comprises at the bottom of silicon wafer-based and magnetic nanoparticle covered with gold leaf, be provided with lattice array at the bottom of described silicon wafer-based to decline pit, described magnetic nanoparticle covered with gold leaf is enriched in described nick hole; Described soft surface strengthens Raman substrate and comprises the hydrogel based end and magnetic nanoparticle covered with gold leaf, is provided with dot matrix column projection the described hydrogel based end, is embedded with described magnetic nanoparticle covered with gold leaf in described projection; Described magnetic nanoparticle covered with gold leaf is the magnetic nanoparticle being coated with layer gold, and described magnetic nanoparticle is iron oxide particle.
By such scheme, the present invention at least has the following advantages: prepare magnetic nanoparticle by hydro-thermal method, regular, that there is uniform particle sizes magnetic nanoparticle covered with gold leaf is prepared subsequently by situ synthesis, and by nick in silicon template hole border physical constraint and regulate and control magnetic nanoparticle covered with gold leaf by magnetic and closely to arrange assembling, significantly improve the mode of SERS hotspot density in unit volume, increase the sensitivity of SERS detection signal, repeatability and homogeneity.This invents the surface enhanced Raman substrate obtained, practical, to have magnetite gathering boundary constraint, lattice array repetition feature, thus provides a kind of novel sensitive SERS detection substrate.This invention is also by magnetite gathering, and the distance between regulation and control iron oxide nanoparticles, obtains the different-effect for surface-enhanced Raman thus.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technological means of the present invention, and can be implemented according to the content of instructions, coordinates accompanying drawing to be described in detail as follows below with preferred embodiment of the present invention.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of 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 scanning electron microscope of magnetic nanoparticle covered with gold leaf in the embodiment of the present invention one;
Fig. 4 is the shape appearance figure by the scanning electron microscope after the method for magnetite gathering micro-pit array at the bottom of silicon wafer-based sprawls nano particle in the embodiment of the present invention one;
Fig. 5 is that soft surface strengthens the shape appearance figure of Raman substrate under optical microscope bright field illumination condition;
Fig. 6 is that in the embodiment of the present invention two, rhodamine R6G adopts hard surface to strengthen the Raman spectrum Comparative result figure of Raman substrate;
Fig. 7 is that in the embodiment of the present invention two, rhodamine R6G adopts soft surface to strengthen the Raman spectrum Comparative result figure of Raman substrate.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Embodiment one
The invention provides a kind of lattice array surface enhanced Raman substrate preparation method, as shown in Figure 1, comprise the following steps successively:
A, prepared the iron oxide particle of uniform particle sizes by hydro-thermal method.
Hydro-thermal method refers to that, in the pressure vessel of sealing, water is solvent, the chemical reaction carried out under the condition of High Temperature High Pressure.Hydro-thermal method be utilize the aqueous solution of High Temperature High Pressure make those in atmospheric conditions insoluble or indissoluble substance dissolves, or reaction generates the lysate of this material, generation convection current is made to separate out the method for grown crystal to form hypersaturated state by the temperature difference controlling solution in autoclave.Concrete preparation method is: 1.08g Iron(III) chloride hexahydrate, 4g anhydrous sodium acetate, under vigorous magnetic stirs, add in the mixed solution of 14mL ethylene glycol and 26mL diethylene glycol, dissolution of solid, the khaki solution obtained.Proceed in the steel bomb of the teflon of three 20mL by this solution mean allocation, sealing is also heated to 200 DEG C in baking oven.React after 15 hours, reactor is placed in room temperature and cools.Respectively with the ferroferric oxide nano granules that water and ethanol purge obtain for twice, vacuum drying 12 hours.
Except hydro-thermal method, sol-gel process also can be adopted to prepare ferriferrous oxide particles, and the method uses Fe
3+, ethanol, ethylene glycol is mixed with colloidal sol, at 300-1000 DEG C, utilize the autoreduction ability of system to obtain ferriferrous oxide film, but the ferriferrous oxide particles poor effect that the method prepares, on product film, particle presents spherical, and having a large amount of crystal defect, particle size is between 40-188nm because heat-treat condition is different.
B, by situ synthesis in iron oxide particle outer cladding layer gold.
In situ synthesis refers to that the method is simple, controlled at next step material of material surface direct growth, and fast can obtain uniform nucleocapsid structure.Also functional group is accessed to connect gold grain by finishing in the method for magnetic nanoparticle outer layer covers gold, but the particle instability that the method is obtained, easily produce functional group and come off, the shortcoming that connection is unstable.By in situ synthesis in iron oxide particle outer cladding layer gold, the firm difficult drop-off of the layer gold obtained and uniform particle sizes.Specific experiment process is as follows:
20mg is dissolved in 5mL tetrahydrofuran, under ultrasonic condition, is slowly instilled in tetrahydrofuran by the 2mL water being dissolved with 20mg dopamine hydrochloride, ultrasonic one hour.Room temperature for overnight put into by mixed liquor.The mode of excessive dopamine Magneto separate removes.The tri-iron tetroxide obtained-dopamine Granular composite is in 20mL water.
Gold is planted and is prepared: classical preparation experiment, 12 μ L 80%THPC and 250 μ L NaOH (2M) join in the deionized water of 45mL successively.Vigorous stirring is after five minutes, 2mL 1% gold chloride be added in above-mentioned solution, lucifuge stirs spends the night.
Gold growth-promoting media: 1.5mL 1% gold chloride joins and is dissolved with in the 100mL deionized water of 25mg sal tartari.After 10 minutes, solution becomes colourless.Growth-promoting media placement is spent the night for subsequent use.
Gold plants absorption: the gold kind of surface band negative charge is adsorbed in the surface of the ferriferrous oxide particles that dopamine is modified by electrostatic interaction.The gold kind solution of 8mL joins the dopamine-tri-iron tetroxide (1mg/mL of 5mL
– 1) in suspending liquid.The acetic acid of 0.2M instills in this growth-promoting media, and pH value of solution is adjusted to about 4.Mixed liquor acutely rocks and spends the night.Excessive gold kind removes by the mode that Magneto separate also cleans.
Layer gold grows: in order to form the golden shell of thick-layer, use the method for this growth in situ.The golden growth-promoting media of 100mL adds dopamine-ferriferrous oxide particles solution (1mg/mL that 5mL has adsorbed golden kind under the condition of vigorous stirring
– 1) in, the formalin with 29%, as reductive agent, is added dropwise in above-mentioned solution, until solution becomes dusty blue.
By in situ synthesis in iron oxide particle outer cladding layer gold, obtained magnetic nanoparticle shaggy covered with gold leaf as shown in Figures 2 and 3, wherein Fig. 2 is the transmission electron microscope photo of magnetic nanoparticle covered with gold leaf, illustrate the nano particle pattern after the coarse layer gold of surface parcel, Fig. 3 is the electron scanning micrograph of gold-covered nano particle, as can be seen from Fig. 2 and Fig. 3, prepare having good uniformity of nano particle, particle diameter is at 138 ran.
C, to prepare by photoetching process there is micro-pit array silicon wafer-based at the bottom of.
Photoetching process utilizes photoimaging and light-sensitive emulsion in substrate as process patterned on the materials such as silicon.Photoetching process due to its design accurately, little, applied widely, the reproducible advantage of error, for designing and producing the process of template.Experimental technique is as follows: use the N-shaped 100 crystal face silicon chip (LuoYang Single CrystalSilicon Co.China) of 4 inches as substrate.Then the ultra-thin aluminium lamination of one deck 300 nanometer is sputtered thereon.Use the technology of ultraviolet photolithographic, by mask plate, the photoresist (RZJ304) of 2 micron thickness on aluminium surface is made pattern again.With nitric acid, unnecessary photoresist is removed, use potassium hydroxide solution to etch aluminium lamination.Using etched aluminium lamination as template, utilize inductively coupled plasma to etch silicon layer, finally can prepare the microarray template of suitable dimension.
Adopt acetone, ethanol and deionized water successively after ultrasonic cleaning at the bottom of d, silicon wafer-based, use nitrogen gun to dry up.
The hydrophilic treatment that plasma washing machine is not less than 1min is put at the bottom of e, silicon wafer-based.
F, as seen in figs. 1 a-1b, under the sucking action of magnet, is enriched in nick hole by magnetic nanoparticle covered with gold leaf;
G, as shown in Figure 1 C, excessive in the magnetic nanoparticle covered with gold leaf in nick hole in cleaning silicon wafer substrate, the hard surface obtained as shown in Figure 4 strengthens Raman substrate, Fig. 4 hard surface nick strengthened in Raman substrate is evenly paved with magnetic nanoparticle covered with gold leaf in cheating, and smooth cleaning outside pit, as shown in figure ip, this hard surface enhancing Raman substrate can do Raman detection to other material under laser.
H, as referring to figure 1e, fills the hydrogel before solidification and covers hard surface and strengthen in Raman substrate;
I, as shown in fig. 1f, after hydrogel solidification, it is peeled off at the bottom of silicon wafer-based, the soft surface obtained as shown in Figure 5 strengthens Raman substrate, circular for displaced gold-covered nano particulate material gel micro-protuberance thereon, present darker color, blank parts is then the smooth pattern-free part of gel.
Wherein, lattice array surface enhanced Raman substrate of the present invention, comprise hard surface and strengthen Raman substrate and soft surface enhancing Raman substrate two kinds of forms, wherein, hard surface strengthens Raman substrate and comprises at the bottom of silicon wafer-based and magnetic nanoparticle covered with gold leaf, be provided with lattice array at the bottom of silicon wafer-based to decline pit, magnetic nanoparticle covered with gold leaf is enriched in nick hole, and hard surface strengthens Raman substrate and is made up of above-mentioned steps a-g; Soft surface strengthens Raman substrate and comprises the hydrogel based end and magnetic nanoparticle covered with gold leaf, is provided with dot matrix column projection the hydrogel based end, is embedded with magnetic nanoparticle covered with gold leaf in projection, and soft surface strengthens Raman substrate and is made up of above-mentioned steps a-i; Magnetic nanoparticle covered with gold leaf is the iron oxide particle being coated with layer gold.
Embodiment two
The invention provides the lattice array surface enhanced Raman substrate in embodiment one, to the rhodamine 6G (10 of variable concentrations
-5m, 10
-6m, 10
-7m) Raman detection result is done.
As shown in Figure 6 and Figure 7, the contrast of the displaying to variable concentrations R6G testing result of hard and soft surface enhanced Raman substrate is respectively; As shown in Figure 6, the boundary constraint lattice array of the hard prepared as surface Raman enhancement substrate to variable concentrations (10
-5, 10
-6, 10
-7m) R6G solution has very strong Raman signal, and its Raman spectrum is at feature peak position 1180,1313,1363,1510,1575 and 1650cm
-1intensity be also apparent, in figure, R6G solid refers to R6G solid, and concentration can regard 1M as, and detectability (LOD) is approximately 10
-7m.As shown in Figure 7, the soft boundary constraint lattice array prepared as surface Raman enhancement substrate to variable concentrations (10
-4, 10
-5) R6G solution have stronger Raman signal, its Raman spectrum is at feature peak position 1180,1313,1363,1510,1575 and 1650cm
-1intensity be also apparent.In figure, R6G solid refers to R6G solid, and concentration can regard 1M as, and detectability (LOD) is approximately 10
-5m.Soft strengthen Raman substrate with hard surface compared with, its detectability (LOD) is higher.
The above is only the preferred embodiment of the present invention; be not limited to the present invention; should be understood that; for those skilled in the art; under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (10)
1. a lattice array surface enhanced Raman substrate preparation method, is characterized in that: comprise the following steps successively:
The magnetic nanoparticle of the metal oxide of a, the iron content preparing uniform particle sizes, cobalt or nickel;
B, in magnetic nanoparticle outer cladding layer gold, obtain magnetic nanoparticle covered with gold leaf;
C, prepare have lattice array decline pit silicon wafer-based at the bottom of;
Dry up after cleaning at the bottom of d, described silicon wafer-based;
E, by hydrophilic treatment at the bottom of described silicon wafer-based;
F, under the sucking action of magnet, magnetic nanoparticle covered with gold leaf is enriched in nick hole in;
Excessive in the magnetic nanoparticle covered with gold leaf in nick hole in g, cleaning silicon wafer substrate, obtain hard surface and strengthen Raman substrate.
2. lattice array surface enhanced Raman substrate preparation method according to claim 1, is characterized in that: in described step a, and described magnetic nanoparticle is iron oxide particle.
3. lattice array surface enhanced Raman substrate preparation method according to claim 1, be is characterized in that: in described step a, is prepared the magnetic nanoparticle of uniform particle sizes by hydro-thermal method.
4. lattice array surface enhanced Raman substrate preparation method according to claim 1, is characterized in that: in described step b, by situ synthesis in magnetic nanoparticle outer cladding layer gold.
5. lattice array surface enhanced Raman substrate preparation method according to claim 1, is characterized in that: in described step c, prepares at the bottom of the silicon wafer-based with micro-pit array by photoetching process.
6. lattice array surface enhanced Raman substrate preparation method according to claim 1, is characterized in that: in described steps d, adopts acetone, ethanol and deionized water successively after ultrasonic cleaning at the bottom of silicon wafer-based, uses nitrogen gun to dry up.
7. lattice array surface enhanced Raman substrate preparation method according to claim 1, is characterized in that: in described step e, puts into the hydrophilic treatment that plasma washing machine is not less than 1min at the bottom of described silicon wafer-based.
8. lattice array surface enhanced Raman substrate preparation method according to claim 1, is characterized in that: also carry out step h and step I after described step a-g, wherein,
H, the hydrogel before solidification filled cover hard surface and strengthen in Raman substrate;
I, until hydrogel solidification after, it is peeled off at the bottom of silicon wafer-based, obtain soft surface strengthen Raman substrate.
9. a lattice array surface enhanced Raman substrate, it is characterized in that: comprise hard surface and strengthen Raman substrate and soft surface enhancing Raman substrate two kinds of forms, wherein, described hard surface strengthens Raman substrate and comprises at the bottom of silicon wafer-based and magnetic nanoparticle covered with gold leaf, be provided with lattice array at the bottom of described silicon wafer-based to decline pit, described magnetic nanoparticle covered with gold leaf is enriched in described nick hole; Described soft surface strengthens Raman substrate and comprises the hydrogel based end and magnetic nanoparticle covered with gold leaf, be provided with dot matrix column projection the described hydrogel based end, be embedded with described magnetic nanoparticle covered with gold leaf in described projection, described magnetic nanoparticle covered with gold leaf is the magnetic nanoparticle being coated with layer gold.
10. lattice array surface enhanced Raman substrate according to claim 9, is characterized in that: described magnetic nanoparticle is iron oxide particle.
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