CN105562936B - A kind of preparation method of the aluminum nanostructured for surface enhanced raman spectroscopy - Google Patents
A kind of preparation method of the aluminum nanostructured for surface enhanced raman spectroscopy Download PDFInfo
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- CN105562936B CN105562936B CN201510982555.5A CN201510982555A CN105562936B CN 105562936 B CN105562936 B CN 105562936B CN 201510982555 A CN201510982555 A CN 201510982555A CN 105562936 B CN105562936 B CN 105562936B
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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
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Abstract
The invention discloses a kind of preparation method of the aluminum nanostructured for surface enhanced raman spectroscopy, first with reguline metal aluminum target as raw material, fully polishes;Then the aluminum target after polishing is placed in chromatographically pure alcoholic environment carries out ultrasound;Aluminum target surface after ultrasound is wiped clean and is placed in the small beaker equipped with liquid nitrogen, keep liquid nitrogen liquid level stabilizing in beaker;Under room temperature, target is taken using millisecond laser straight by the assosting effect for carrying electric displacement platform, the patterning of nanostructured is realized.Instant invention overcomes the repeated bad problem of existing preparation technology apparatus expensive, complex process, and reinforcement.The simple synthesis of aluminum nanostructured reinforcement is realized in liquid nitrogen environment at normal temperatures and pressures, more dense Raman focus is obtained, is drastically increased the sensitivity of detection.Synthetic method of the present invention is simple, easy to operate, reproducible, and the detectivity to detecting thing molecule is high, and belongs to normal temperature and pressure synthesis, environmental protection, is a kind of eco-friendly green synthesis process.
Description
Technical field
The present invention relates to a kind of preparation method of aluminum nanostructured, the more particularly to aluminum for surface enhanced raman spectroscopy is received
The preparation method of rice structure.
Background technology
In recent years, LSPR phenomenons due to its unique optical property and its fields such as biological medicine, food safety weight
To apply and get more and more people's extensive concerning.The nanostructured of metal surface is subject to the effect of incident illumination to excite plasma resonance existing
As, the enhanced electric field of local is produced, the electric field height local is in nanostructured surface, the main shape for being subject to nano structured unit
Distance between shape, size, residing media environment and construction unit etc. is controlled, referring to:Lim, D.-K, Jeon, K-S and
Suh, Y.D, Nat.Mater.2010,9,60-67.The LSPR of this structure and condition depended is successfully applied to surface
Strengthen Raman spectrum (SERS) and surface-enhanced fluorescence spectrum (SEF).So-called SERS is precisely due to the notable increasing of LSPR generations
Strong local electric field is affected so that the Raman spectrum that raman scattering cross section is greatly improved, and what electric field was significantly increased
Position is normally referred to as Raman focus, is predominantly located at metal Nano structure (nanocluster etc.) less gap and nanotip
Position, and the scattering section for detecting thing molecule in hotspot location can be presented the enhancing phenomenon of several orders of magnitude, it might even be possible to reach
To monomolecular detection level, referring to:Talley, C.E, Jackson, J.B and Oubre, C, NanoLett.2005,5,
1569–1574。
The Raman spectrum that ultraviolet light (UV) is excited has been applied to the detection of many Organic substances and inorganic matters.Additionally, grinding
The fluorescence signal for finding many biomolecule is studied carefully mostly in visible region, and fluorescence can be prevented effectively from using uv excitation light
The interference problem of signal.As the scattering section in Raman spectrum, detecting thing molecule is proportional to the biquadratic of incident light frequency, institute
The signal to noise ratio that Raman can be lifted is excited with ultraviolet light (UV), referring to:Asher,S.A and Johnson,C.R,Science
1984,225,311.And the biomolecule such as DNA has absorption band in ultraviolet light, resonance Raman effect can be produced with incident illumination, most
Cause Raman signal to obtain further lifting eventually and even can reach 108 orders of magnitude, referring to:Shankar K.Jha and
Zeeshan Ahmed,J.Am.Chem.Soc.2012,134,1966-1969。
The enhancing substrate for being presently used for SERS researchs is concentrated mainly on visible region, research be concentrated mainly on gold and
Silver, but due to its visible-range have absorption and high cost and relatively low resource reserve significantly limit its application.
Compared to gold and silver, aluminium surface goes out more significant ground plasma resonance phenomenon, and which has to ultraviolet light near 200nm significantly inhales
Receive and LSPR is adjustable for height from ultraviolet light to visible region.But, LSPR is for the oxidation of aluminum metal nanostructured
And the distance between nano structured unit is very sensitive, degree of oxidation is bigger, more remote its LSPR of the distance between construction unit
Produced electric-field enhancing is weaker, ultimately results in the hydraulic performance decline of SERS.In order to obtain preferable Raman signal, it should meet with
Lower requirement (1), the performance of Nano-cluster configuration are better than single nanoparticle (2), are prevented effectively from the internal oxidation (3) of granule, receive
The distance between rice construction unit is as far as possible little, and the phenomenon of dense distribution is presented.Current research method mainly has, such as photoetching process
The metal Nano structure of high-sequential is prepared, although which obviating the internal oxidation problem of granule, between construction unit
It is distant, cause electric-field enhancing unobvious, corresponding Raman focus is also just very rare;The also method system of nano impression
For equally orderly nanostructured, but construction unit size is equally faced greatly with photoetching process, Raman focus is few, and equipment is held high
It is expensive, the harsh problem of experiment condition, referring to:Tao Ding and Daniel O.Sigle,ACS
Appl.Mater.Interfaces 2014,6,17358-17363.As the preparation method of this traditional aluminum nanostructured, example
Such as photoetching, nano impression, molecular beam epitaxy etc., are subjected to the restriction of the conditions such as apparatus expensive, experiment condition harshness, so as to limit
The extensive application of LSPR is made.
In this numerous synthetic method, it is that a kind of simple, quick, low cost is prepared and received that laser directly inscribes method (LDW)
The method of rice structure.Millisecond laser ablation aluminum is adopted under the assosting effect of electric displacement platform by the restriction effect that rapidly cools down of liquid nitrogen
Target, quickly prepares on the surface of aluminum target and is smaller in size than 100nm aluminum clusters arrays, and which has in UV light region and significantly absorbs.This
The nanostructured meeting surface for planting surface dense distribution goes out preferable SERS performances and highdensity Raman focus, and either strengthens
Body or signal can all show fabulous repeatability.So far, aluminum nanoparticles structure is quickly, simply prepared as this
Method also do not reported.
The content of the invention
In order to solve problems of the prior art, the present invention provides a kind of aluminum for surface enhanced raman spectroscopy and receives
The preparation method of rice structure, prepares the method complex process of SERS reinforcements, apparatus expensive and repeatability in overcoming prior art
Also bad problem.
The technical scheme is that:A kind of preparation method of the aluminum nanostructured for surface enhanced raman spectroscopy, bag
Include following steps:
(1) with reguline metal aluminum target as raw material, before laser target shooting, fully polish, fully remove surface oxidation to reach
Layer and reach the closely smooth purpose in surface;
(2) the aluminum target after polishing is placed in chromatographically pure alcoholic environment carries out ultrasound;
(3) the aluminum target surface after ultrasound is wiped clean and is placed in the small beaker equipped with liquid nitrogen, keep liquid nitrogen liquid level in beaker
It is stable;
(4), under room temperature, target is taken using millisecond laser straight by the assosting effect for carrying electric displacement platform, the figure of nanostructured is realized
Case;
(5) the nanostructured reinforcement that preparation is finished is put in the crystal violet aqueous solution of variable concentrations and is soaked, take out sample
Product are stood to sample surfaces does not have liquid that Raman test is proceeded by when flowing.
The step (1) fully polishing refers to the surface of aluminum of first fully being polished with the sand paper of different model, then uses 50nm
Alumina powder polished again.
The liquid level of step (3) liquid nitrogen maintains 1-2.5cm.Small beaker be placed in the thermos cup equipped with liquid nitrogen with
Keep liquid nitrogen liquid level stabilizing in beaker.
The aluminum target purity is 99.995%, and its thickness is 2mm.
When step (4) the millisecond laser straight takes target, the energy of laser is 2.227J, and laser repetition rate is 1HZ.Swash
It is 5-10mL that light adds amount of liquid nitrogen every 6min during practicing shooting, to maintain the liquid level of target upper surface.
Step (5) soak time is 18h.
Beneficial effects of the present invention are:The present invention directly sputters the aluminum target in liquid nitrogen environment using millisecond laser, by swashing
The ablation effect of light directly sputters the nano-particle or Cluster Structures for producing small size (10-100nm) in target material surface, due to
Nanostructured is directly connected with substrate, drastically increases the repeatability of Reinforcement structure and the sensitivity of detection;The present invention
The aluminum nanostructured that can be used in high sensitivity UV-SERS is quickly prepared using millisecond laser one-step method, existing system is overcome
Standby process equipment is expensive, complex process, and the repeated bad problem of reinforcement.It is real in liquid nitrogen environment at normal temperatures and pressures
The simple synthesis of aluminum nanostructured reinforcement is showed, has obtained more dense Raman focus, drastically increase the sensitive of detection
Degree.Additionally, synthetic method of the present invention is simple, easy to operate, reproducible, the detectivity to detecting thing molecule
Height, and belong to normal temperature and pressure synthesis, environmental protection, it is a kind of eco-friendly green synthesis process.
Description of the drawings
Experimental equipment used by Fig. 1 present invention;
The nano-particle distribution situation inside application point after Fig. 2 single-pulse lasers one point of effect;(a) laser action
Low power scanning electron microscope diagram piece afterwards;The high power scanning electron microscope of diverse location inside (b), (c), (d) application point
Picture;
Fig. 3 is the three-dimensional appearance of target material surface after laser action;Target pattern after (a) laser action;B () and (c) are not
The three-dimensional appearance of ipsilateral;
The sign of laser action product under Fig. 4 (a) (b) different amplification;The X-ray diffraction of (c) laser action product
Picture;The transmission electron micrograph of (d) laser action product;
Fig. 5 (a) is the absorption picture of the aluminum nanostructured prepared under different liquid levels;B () is under different liquid levels
The Raman picture of the aluminum nanostructured of preparation;Scanned picture of (c) liquid level for the aluminum nanostructured of 1-1.5cm;(d) liquid level
The scanned picture of nanostructured when scanned picture (e) liquid level of nanostructured is 2-2.5cm when being highly 1.5-2cm
Wherein 1- milliseconds focus on light;2- liquid nitrogen;3- aluminum targets;4- electric displacement platforms.
Specific embodiment
With reference to the accompanying drawings and detailed description the present invention is elaborated.
The sand paper of the pure aluminum target sand for surface paper different model of 20 × 20 × 3mm (first with coarse sandpaper, then is used into fine sand now
Paper) surface of target is sufficiently polished, effectively to remove the oxide layer on surface, carry out in the alumina powder with 50nm
Polishing, with reach surface try one's best flat smooth purpose.Finally the target after polishing is placed in big centrifuge tube carry out it is repeatedly many
Secondary ultrasound, reaches the purpose of crystallization with the soil for removing surface, and in order to be effectively prevented from the oxidation of target material surface, ultrasound is adopted
Be chromatographically pure ethanol solution.
After ultrasound, the aluminum target that purity is 99.995%, thickness 3mm is placed in the beaker equipped with liquid nitrogen, while by beaker
It is placed in thermos cup to ensure that liquid nitrogen environment is stablized in beaker, prevents the violent boiling of liquid nitrogen.Using millisecond pulse Nd:YAG
Laser (fundamental frequency 1064nm) focuses on photoirradiation target surface, and laser energy is 2.227J, repetition rate 1Hz.By the auxiliary of electric displacement platform
Effect is practiced shooting.Specific experimental provision is as shown in Figure 1.
Before the patterning of nanostructured is realized, the nanostructured for first having to determine obtained by us be dense distribution in
Inside laser action point, so we observe the nanostructured of diverse location inside laser action point simultaneously, such as Fig. 2 institutes
Show.A () is the low power scanning of laser action point, (b) centered on position scanning, (c), (d) figure off center position progressively.
It can be seen that nanostructured does not have too big change in the size and pattern of the diverse location of laser action point, being completely can be with
It is the preparation of first large area, highdensity aluminum nanostructured by the assosting effect of electric displacement platform.
For vivider specific observation, Fig. 3 shows that the target material surface pattern obtained under the assosting effect of electric displacement platform is
By the preiodic type structure for necessarily rising and falling, there is groove, the corresponding center for being to focus on light in this structure.In order to prove us
Without being oxidized in laser action process, Fig. 4 (c), (d) sets forth the x of aluminum nanostructured to the aluminum nanostructured of preparation
X ray diffration pattern x and high resolution transmission electron microscope picture.Do not see in Fig. 4 (c) that the diffraction maximum of aluminium oxide illustrates me
Product be aluminum, the high power transmission electron micrograph of Fig. 4 (d) points out that laser action product is that the aluminum containing oxide layer is received
The nucleocapsid structure of rice grain, the surface of aluminum nanoparticles is amorphous oxide layer, and thickness is in 2.5nm or so.
Further we also explore the impact of the liquid level for Raman spectrum of liquid nitrogen.Obtain on height too high target surface
Obtaining effective laser energy reduces, and target can not be by effectively ablation, and the ablated phenomenon of the too low target material surface of liquid level is serious,
Both of these case can all cause the reduction of nanostructured, Raman hydraulic performance decline.Fig. 5 mainly discusses liquid level for 1-2.5cm
Optimum capacity scope, either from pattern, absorb or Raman spectrum, can draw their performance be all it is consistent,
1-2.5cm is optimal liquid level scope.A () figure is the absorption picture under different liquid levels, its Raman figure with (b) figure
And the shape appearance figure of (c) (d) (e) all shows, these three liquid levels are optimum liquid levels, and its Raman performance is consistent
's.
In Raman test process, material is had significant effect for performance in the state of target material surface, if there is water on surface
Mobility then fluorescence signal is too strong;Dry tack free, Raman signal are also bad, so will ensure target material surface half in test process
The wet half-dried state for not having liquid flowing carries out Raman test.
Although above in conjunction with accompanying drawing, invention has been described, the invention is not limited in above-mentioned being embodied as
Mode, above-mentioned specific embodiment is only schematic, is not restricted, and one of ordinary skill in the art is at this
Under the enlightenment of invention, in the case of without departing from present inventive concept and scope of the claimed protection, many shapes can also be made
Formula, these are belonged within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of the aluminum nanostructured for surface enhanced raman spectroscopy, it is characterised in that comprise the following steps:
(1), with reguline metal aluminum target as raw material, before laser target shooting, fully polish, with reach fully remove surface oxide layer with
And reach the closely smooth purpose in surface;
(2) the aluminum target after polishing is placed in chromatographically pure alcoholic environment carries out ultrasound;
(3) the aluminum target surface after ultrasound is wiped clean and is placed in the small beaker equipped with liquid nitrogen, keep liquid nitrogen liquid level stabilizing in beaker;
(4), under room temperature, target is taken using millisecond laser straight by the assosting effect for carrying electric displacement platform, the pattern of nanostructured is realized
Change;
(5) the nanostructured reinforcement that preparation is finished is put in the crystal violet aqueous solution of variable concentrations and is soaked, take out sample quiet
Putting to sample surfaces does not have liquid that Raman test is proceeded by when flowing.
2. the preparation method of the aluminum nanostructured of surface enhanced raman spectroscopy is used for according to claim 1, it is characterised in that
The step (1) fully polishing refers to the surface of aluminum of first fully being polished with the sand paper of different model, then with the aluminium oxide of 50nm
Powder is polished again.
3. the preparation method of the aluminum nanostructured of surface enhanced raman spectroscopy is used for according to claim 1, it is characterised in that
The liquid level of step (3) liquid nitrogen maintains 1-2.5cm.
4. the preparation method of the aluminum nanostructured of surface enhanced raman spectroscopy is used for according to claim 1, it is characterised in that
Step (3) small beaker is placed in the thermos cup equipped with liquid nitrogen to keep liquid nitrogen liquid level stabilizing in beaker.
5. the preparation method of the aluminum nanostructured of surface enhanced raman spectroscopy is used for according to claim 1, it is characterised in that
The aluminum target purity is 99.995%, and its thickness is 2mm.
6. the preparation method of the aluminum nanostructured of surface enhanced raman spectroscopy is used for according to claim 1, it is characterised in that
When step (4) the millisecond laser straight takes target, the energy of laser is 2.227J, and laser repetition rate is 1HZ.
7. the preparation method of the aluminum nanostructured of surface enhanced raman spectroscopy is used for according to claim 1, it is characterised in that
It is 5-10mL to add amount of liquid nitrogen every 6min during step (4) laser target shooting, to maintain the liquid level of target upper surface high
Degree.
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CN107598155B (en) * | 2017-09-08 | 2019-08-23 | 中国科学院合肥物质科学研究院 | The preparation method of lead nano particle |
CN108436253B (en) * | 2018-02-26 | 2020-07-17 | 北京航空航天大学 | Preparation method of SERS-fluorescence dual-mode metal enhanced substrate |
CN113560712B (en) * | 2021-07-14 | 2022-11-25 | 北京理工大学 | Method for preparing two-dimensional material nanostructure through ultrafast laser processing |
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