CN105562936A - Preparation method of aluminum nanometer structure for surface enhancement of Raman scattering - Google Patents
Preparation method of aluminum nanometer structure for surface enhancement of Raman scattering Download PDFInfo
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- CN105562936A CN105562936A CN201510982555.5A CN201510982555A CN105562936A CN 105562936 A CN105562936 A CN 105562936A CN 201510982555 A CN201510982555 A CN 201510982555A CN 105562936 A CN105562936 A CN 105562936A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/36—Removing material
- B23K26/361—Removing material for deburring or mechanical trimming
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Abstract
The invention discloses a preparation method of an aluminum nanometer structure for surface enhancement of Raman scattering. Firstly, a bulk metal aluminum target serves as a raw material for full polishing; then, the polished aluminum target is put in a chromatographically pure ethanol environment for ultrasound treatment; the surface of the aluminum target subjected to ultrasound treatment is cleaned; the aluminum target is put in a small beaker with liquid nitrogen; the liquid level of the liquid nitrogen in the beaker is kept stable; and at normal temperature, the direct target shootingis performed by using millisecond laser by dint of auxiliary effect of lifting an electric displacement table to realize patterning of the nanometer structure. According to the preparation method,the problems of expensive equipment, complex process and weak repeatability of a reinforcement body in a traditional preparation process are overcome, simple synthesis of the reinforcement body of the aluminum nanometer structure in the liquid nitrogen environment with normal temperature and normal pressure is realized, denser Raman hot spots are obtained, and the detecting sensitivity is greatly improved. The preparation method is simple in synthesis method, convenient for operation, excellent in repeatability and high in detecting sensitivity of detected object molecules, belongs to normal-temperature and normal-pressure synthesis, is green and environment-friendly, and is an environment-friendly green synthesis process.
Description
Technical field
The present invention relates to a kind of preparation method of aluminium nanostructured, particularly for the preparation method of the aluminium nanostructured of SERS.
Background technology
In recent years, LSPR phenomenon is due to the optical property of its uniqueness and it is in biological medicine, the important application in the fields such as food security and getting more and more people's extensive concerning.The effect that the nanostructured of metal surface is subject to incident light excites plasma resonance phenomenon, produce the electric field that local strengthens, this electric field height local, at nanostructured surface, is mainly subject to the controls such as the distance between the shape of nano structured unit, size, residing media environment and construction unit, see: Lim, D.-K, Jeon, K-SandSuh, Y.D, Nat.Mater.2010,9,60-67.The LSPR of this structure and condition depended has successfully been applied to SERS (SERS) and surface-enhanced fluorescence spectrum (SEF).So-called SERS is exactly because the local electric field of the remarkable enhancing of LSPR generation affected, make the Raman spectrum that raman scattering cross section is greatly improved, and the position that electric field significantly strengthens is referred to as Raman focus usually, mainly be positioned at the less gap of metal Nano structure (nanocluster etc.) and nanotip position, and the enhancing phenomenon of several order of magnitude can be presented at the scattering section of hotspot location detection thing molecule, even can reach monomolecular detection level, see: Talley, C.E, Jackson, J.BandOubre, C, NanoLett.2005, 5, 1569 – 1574.
The Raman spectrum that ultraviolet light (UV) excites has been applied to the detection of many organic matters and inorganic matter.In addition, research finds that the fluorescence signal of many biomolecule is mostly in visible region, and adopts uv excitation light effectively can avoid the interference problem of fluorescence signal.Due in Raman spectrum, the scattering section of detection thing molecule is proportional to the biquadratic of incident light frequency, so ultraviolet light (UV) excites the signal to noise ratio that can promote Raman, see: Asher, S.AandJohnson, C.R, Science1984,225,311.And the biomolecule such as DNA have absorption band at ultraviolet light, resonance Raman effect can be produced with incident light, finally make Raman signal further be promoted and even can reach 108 orders of magnitude, see: ShankarK.JhaandZeeshanAhmed, J.Am.Chem.Soc.2012,134,1966-1969.
At present, for SERS research enhancing substrate mainly concentrate on visible region, research mainly concentrate on gold and silver, but due to its visible-range have absorption and high cost and lower resource reserve significantly limit its application.Compared to golden and silver-colored, aluminium surface goes out plasma resonance phenomenon more significantly, and it near 200nm, have absorption significantly to ultraviolet light and LSPR is adjustable for height from ultraviolet light to visible region.But LSPR is very responsive for the distance between the oxidation of aluminum metal nanostructured and nano structured unit, and degree of oxidation is larger, and the electric-field enhancing that its LSPR far away of the distance between construction unit produces is more weak, finally causes the hydraulic performance decline of SERS.In order to obtain good Raman signal, following requirement (1) should be met, the performance of Nano-cluster configuration is better than single nanoparticle (2), effectively avoid the distance between the internal oxidation of particle (3), nano structured unit as far as possible little, present the phenomenon of dense distribution.Current research method mainly contains, as photoetching process prepares the metal Nano structure of high-sequential, although which obviate the internal oxidation problem of particle, distant between construction unit, cause electric-field enhancing not obvious, corresponding Raman focus is also with regard to rareness very; The method of nano impression is also had to prepare same orderly nanostructured, but and photoetching process to face construction unit size equally large, Raman focus is few, apparatus expensive, the problem of experiment condition harshness, see: TaoDingandDanielO.Sigle, ACSAppl.Mater.Interfaces2014,6,17358-17363.The restriction of the conditions such as the preparation method of this traditional aluminium nanostructured, such as photoetching, nano impression, molecular beam epitaxy etc., all will be subject to apparatus expensive, and experiment condition is harsh, thus limit the extensive use of LSPR.
In the synthetic method that these are numerous, laser directly inscribe method (LDW) be a kind of simple, fast, low cost prepares the method for nanostructured.The effect of cooling limitation rapidly by liquid nitrogen adopts millisecond laser ablation aluminium target under the booster action of electric displacement platform, is less than 100nm aluminium clusters arrays at the quick preparation size in the surface of aluminium target, and it has in UV light region and absorbs significantly.The nanostructured of this surperficial dense distribution can go out good SERS performance and highdensity Raman focus in surface, and is that reinforcement or signal all can show fabulous repeatability.So far, also do not report to some extent as this method preparing aluminum nanoparticles structure fast, simply.
Summary of the invention
In order to solve problems of the prior art, the invention provides a kind of preparation method of the aluminium nanostructured for SERS, overcoming in prior art the method complex process preparing SERS reinforcement, apparatus expensive and the also bad problem of repeatability.
Technical scheme of the present invention is: a kind of preparation method of the aluminium nanostructured for SERS, comprises the following steps:
(1) with reguline metal aluminium target for raw material, before laser target shooting, fully polish, fully remove surface oxide layer to reach and reach the closely level and smooth object in surface;
(2) the aluminium target after polishing being placed in chromatographically pure alcoholic environment carries out ultrasonic;
(3) small beaker being placed in and liquid nitrogen is housed is wiped clean on the aluminium target surface after ultrasonic, keep liquid nitrogen liquid level stabilizing in beaker;
(4), under normal temperature, adopt millisecond laser straight to play target by the booster action carrying electric displacement platform, realize the patterning of nanostructured;
(5) the crystal violet aqueous solution complete nanostructured reinforcement of preparation being put into variable concentrations soaks, and taking-up sample leaves standstill and do not start to carry out Raman test when sample surfaces has liquid flow.
Described step (1) fully polishing refers to the surface of aluminium of first fully polishing with the sand paper of different model, then polishes with the alumina powder of 50nm again.
The liquid level of described step (3) liquid nitrogen maintains 1-2.5cm.Small beaker be placed in liquid nitrogen is housed thermos cup to keep liquid nitrogen liquid level stabilizing in beaker.
Described aluminium target purity is 99.995%, and its thickness is 2mm.
When described step (4) millisecond laser straight plays target, the energy of laser is 2.227J, and laser repetition rate is 1HZ.In laser target shooting process every 6min annex solution nitrogen quantity be 5-10mL, to maintain the liquid level of target upper surface.
Described step (5) soak time is 18h.
Beneficial effect of the present invention is: the present invention adopts millisecond laser directly to sputter aluminium target in liquid nitrogen environment, directly produced nano particle or the Cluster Structures of small size (10-100nm) in target material surface sputtering by the ablation effect of laser, because nanostructured is directly connected with substrate, drastically increase the repeatability of Reinforcement structure and the sensitivity of detection; The present invention utilizes millisecond laser one-step method to prepare the aluminium nanostructured that can be used in high sensitivity UV-SERS fast, overcomes existing preparation technology's apparatus expensive, complex process, and the problem that the repeatability of reinforcement is bad.Achieve the simple synthesis of aluminium nanostructured reinforcement in liquid nitrogen environment at normal temperatures and pressures, obtain more intensive Raman focus, drastically increase the sensitivity of detection.In addition, synthetic method of the present invention is simple, easy and simple to handle, reproducible, high to the detectivity of detection thing molecule, and belongs to normal temperature and pressure synthesis, environmental protection, is a kind of eco-friendly green synthesis process.
Accompanying drawing explanation
Fig. 1 the present invention Experimental equipment used;
The nano particle distribution situation of the application point inside after Fig. 2 single-pulse laser effect point; Low power scanning electron microscope diagram sheet after (a) laser action; The high power scanning electron microscope diagram sheet of (b), (c), the inner diverse location of (d) application point;
Fig. 3 is the three-dimensional appearance of target material surface after laser action; Target pattern after (a) laser action; The three-dimensional appearance of (b) and (c) not ipsilateral;
The sign of laser action product under Fig. 4 (a) (b) different amplification; The X-ray diffraction picture of (c) laser action product; The transmission electron micrograph of (d) laser action product;
The absorption picture of aluminium nanostructured of Fig. 5 (a) for preparing under different liquid level; (b) Raman picture of aluminium nanostructured for preparing under different liquid level; C () liquid level is the scanned picture of the aluminium nanostructured of 1-1.5cm; The scanned picture of nanostructured when scanned picture (e) liquid level of nanostructured is 2-2.5cm when () liquid level is 1.5-2cm d
Wherein 1-millisecond focused light; 2-liquid nitrogen; 3-aluminium target; 4-electric displacement platform.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is elaborated.
Now the sand paper of the pure aluminum target sand for surface paper different model of 20 × 20 × 3mm (is first used coarse sandpaper, use fine sandpaper again) polished fully in the surface of target, effectively to remove the oxide layer on surface, polishing with the alumina powder of 50nm, to reach the object of surperficial flat smooth as far as possible.Finally the target after polishing is placed in large centrifuge tube and carries out repeated multiple times ultrasonic, reach the object of crystallization with the dirt removing surface, in order to effectively avoid the oxidation of target material surface, ultrasonic employing be chromatographically pure ethanolic solution.
After ultrasonic, be 99.995% by purity, the aluminium target of thickness 3mm is placed in the beaker that liquid nitrogen is housed, beaker is placed in thermos cup to ensure the stable of beaker liquid nitrogen environment simultaneously, prevents the violent boiling of liquid nitrogen.Adopt millisecond Pulse Nd: YAG laser (fundamental frequency 1064nm) focused light irradiation target surface, laser energy is 2.227J, repetition rate 1Hz.Booster action by electric displacement platform is practiced shooting.Concrete experimental provision as shown in Figure 1.
Before realizing the patterning of nanostructured, first to determine nanostructured that we obtain be dense distribution in laser action point inside, so we observe the nanostructured of the inner diverse location of laser action point simultaneously, as shown in Figure 2.A () is the low power scanning of laser action point, the scanning of position centered by (b), (c), (d) figure off center position progressively.Can find out that nanostructured does not have too large change in the size of the diverse location of laser action point and pattern, be can be the preparation of first large area, highdensity aluminium nanostructured completely by the booster action of electric displacement platform.
In order to vivider observation specifically, Fig. 3 shows that the target material surface pattern obtained under the booster action of electric displacement platform is that this structure exists groove by the preiodic type structure necessarily risen and fallen, the center of corresponding is focused light.In order to prove that the aluminium nanostructured that we prepare does not have oxidized in laser action process, Fig. 4 (c), (d) sets forth x-ray diffraction pattern and the high resolution transmission electron microscope picture of aluminium nanostructured.Do not see in Fig. 4 (c) that the diffraction maximum of aluminium oxide illustrates that our product is aluminium, the high power transmission electron micrograph of Fig. 4 (d) points out that laser action product is the nucleocapsid structure of the aluminum nanoparticles containing oxide layer, the surface of aluminum nanoparticles is amorphous oxide layer, and thickness is at about 2.5nm.
We also explore the impact of liquid level for Raman spectrum of liquid nitrogen further.Highly too high target surface obtains effective laser energy and reduces, and target can not by ablation effectively, and the ablated phenomenon of the too low target material surface of liquid level is serious, and both of these case all can cause the minimizing of nanostructured, Raman hydraulic performance decline.Fig. 5 mainly discusses the optimum capacity scope that liquid level is 1-2.5cm, no matter is from pattern, absorption or Raman spectrum, can show that their performance is all consistent, and 1-2.5cm is best liquid level scope.A () figure is the absorption picture under different liquid level, it all demonstrates with the Raman figure of (b) figure and the shape appearance figure of (c) (d) (e), these three liquid levels are optimum liquid levels, and its Raman performance is consistent.
In Raman test process, material has great impact in the state of target material surface for performance, if there is the mobility of water on surface, fluorescence signal is too strong; Dry tack free, Raman signal is also bad, does not half-driedly have the state of liquid flow to carry out Raman test so will ensure in test process that target material surface half is wet.
Although invention has been described by reference to the accompanying drawings above; but the present invention is not limited to above-mentioned detailed description of the invention; above-mentioned detailed description of the invention is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; do not departing under the ambit that present inventive concept and claim protect, can also make a lot of form, these all belong within protection scope of the present invention.
Claims (8)
1., for a preparation method for the aluminium nanostructured of SERS, it is characterized in that, comprise the following steps:
(1) with reguline metal aluminium target for raw material, before laser target shooting, fully polish, fully remove surface oxide layer to reach and reach the closely level and smooth object in surface;
(2) the aluminium target after polishing being placed in chromatographically pure alcoholic environment carries out ultrasonic;
(3) small beaker being placed in and liquid nitrogen is housed is wiped clean on the aluminium target surface after ultrasonic, keep liquid nitrogen liquid level stabilizing in beaker;
(4), under normal temperature, adopt millisecond laser straight to play target by the booster action carrying electric displacement platform, realize the patterning of nanostructured;
(5) the crystal violet aqueous solution complete nanostructured reinforcement of preparation being put into variable concentrations soaks, and taking-up sample leaves standstill and do not start to carry out Raman test when sample surfaces has liquid flow.
2. according to claim 1 for the preparation method of the aluminium nanostructured of SERS, it is characterized in that, described step (1) fully polishing refers to the surface of aluminium of first fully polishing with the sand paper of different model, then polishes with the alumina powder of 50nm again.
3. according to claim 1 for the preparation method of the aluminium nanostructured of SERS, it is characterized in that, the liquid level of described step (3) liquid nitrogen maintains 1-2.5cm.
4., according to claim 1 for the preparation method of the aluminium nanostructured of SERS, it is characterized in that, described step (3) small beaker be placed in liquid nitrogen is housed thermos cup to keep liquid nitrogen liquid level stabilizing in beaker.
5., according to claim 1 for the preparation method of the aluminium nanostructured of SERS, it is characterized in that,
Described aluminium target purity is 99.995%, and its thickness is 2mm.
6. according to claim 1 for the preparation method of the aluminium nanostructured of SERS, it is characterized in that, when described step (4) millisecond laser straight plays target, the energy of laser is 2.227J, and laser repetition rate is 1HZ.
7. according to claim 1 for the preparation method of the aluminium nanostructured of SERS, it is characterized in that, in described step (4) laser target shooting process every 6min annex solution nitrogen quantity be 5-10mL, to maintain the liquid level of target upper surface.
8. according to claim 1 for the preparation method of the aluminium nanostructured of SERS, it is characterized in that, described step (5) soak time is 18h.
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| CN107598155A (en) * | 2017-09-08 | 2018-01-19 | 中国科学院合肥物质科学研究院 | Lead nano particle and preparation method thereof |
| CN108436253A (en) * | 2018-02-26 | 2018-08-24 | 北京航空航天大学 | A kind of preparation method of SERS- fluorescent dual modules formula metal enhancing substrate |
| CN113560712A (en) * | 2021-07-14 | 2021-10-29 | 北京理工大学 | Method for preparing two-dimensional material nanostructure by ultrafast laser processing |
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