CN109112598A - A kind of method of iron nano-dot matrix auxiliary preparation self assembly strawberry-like gold SRES substrate - Google Patents
A kind of method of iron nano-dot matrix auxiliary preparation self assembly strawberry-like gold SRES substrate Download PDFInfo
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Abstract
The present invention relates to a kind of methods that iron nano-dot matrix assists preparation self assembly strawberry-like gold SRES substrate, and steps are as follows: preparing the AAO template of uniform pore diameter, Fe nanowire is then grown in AAO template, forms the strawberry-like gold nano dot matrix of marshalling after gold-plated.Compared with prior art, the present invention has the advantages that the present invention has, preparation is simple, synthesis process is efficiently succinct, pollution-free, and feature at low cost, using being formed on Fe nanowire during vapor deposition, large area is regular, structure-controllable, high sensitivity, the self assembly Au nanosphere array structure of the strawberry-like formd, the SERS substrate of this self assembly can form the nano-array on coarse surface and marshalling, there is very high Raman enhancing activity, it can reuse, the stability for improving SERS, can be widely applied in trace detection.
Description
Technical field
The present invention relates to a kind of preparation methods of metal nano array substrate, and in particular to a kind of iron nano-dot matrix auxiliary system
The method of standby self assembly strawberry-like gold SRES substrate.
Background technique
With the progress of science and technology, orderly noble metal nano array is more and more closed with its unique performance
Note, related research result obtain in fields such as surface Raman enhancement (SERS) substrate, solar battery, micro-nano opto-electronic devices
It is widely applied.In numerous precious metal materials, golden (Au) is widely used in metal Nano structure battle array because of its excellent performance
The preparation and research of column.The performance of metal Nano structure depends primarily on local surface plasma resonance (LSPR), and also and its
The relevant parameters such as size, the form of nanostructure are closely coupled.Therefore, efficient preparation and the spy of metal nano array how to be realized
The flexible modulation of different morphology and size, and effectively reduce cost be the research of metal nano array one of main problem.
Up to the present, there has been proposed it is a variety of it is micro-, receive processing precise method, realize the system of various metal nano arrays
Standby and structure size control method, wherein most exemplary process is mainly lithographic method and template, such as photoetching, electron beam
Etching etc..Although these a variety of methods have precision higher, processing efficiency is low, at high cost, is unfavorable for large scale, scale system
The problems such as sample, constrain it is micro-, receive metal structure and miniature device preparation in application.
Surface enhanced Raman scattering (SERS) is one of widely applied example of metal nano array, since it may be implemented
Micro quick detection can ensure that the food safety of people, thus all be widely used in diverse discipline field, wherein leading
It is related to the development fields such as biology, chemistry, analytical chemistry and detection organic content.SERS enhancement effect, mainly from substrate
Roughening metal surfaces electromagnetism mechanism and solved to two aspects of the relevant chemical mechanism of the binding molecule of effect are generated
It releases.Therefore, the reinforcing effect that improve SERS first has to the nanometer performance for improving substrate.The lining that traditional production method is produced
Bottom to form the nano-dot matrix being evenly distributed due to being not easy, and test result is unstable；And that there are processes is cumbersome for traditional preparation method,
The problems such as preparation cost is higher, these problems all significantly limit the development that SERS is used as trace detection tool.Therefore, it prepares
Stablize, inexpensive nano-array is micro-, micro-nano structure as substrate is the essential step for pushing SERS to develop.
Summary of the invention
The technical problem to be solved by the invention for the present situation of prior art is to provide a kind of simple processes, production effect
The method of the high and at low cost iron nano-dot matrix auxiliary preparation self assembly strawberry-like gold SRES substrate of rate, the SRES substrate knot of preparation
Structure is controllable, stability is good, reusable.
The technical scheme of the invention to solve the technical problem is: a kind of iron nano-dot matrix auxiliary preparation self assembly
The method of strawberry-like gold SRES substrate, it is characterised in that the following steps are included:
1) the AAO template of 60~80nm of aperture is prepared by anodizing；
2) the AAO template by step 1) preparation cleans impurity elimination, keeps surfacing clean；
3) the electroless deposition Fe nanowire in AAO template: 0.9~1.2mol/L solution of ferrous chloride is prepared, no electricity is passed through
Iron nanometer rods are deposited, grow it according to the aperture of AAO template；It is dry that it is put into vacuum oven after deposition, obtains rule
The iron nanometer stick array of arrangement；
4) gold is deposited in AAO template: using Vacuum Coating method, gold particle is plated in step 3) system in the environment of vacuum
In the AAO template of the iron nanometer stick array obtained, the substrate with Au nanometers of ball arrays of strawberry-like is obtained.
Preferably, the specific preparation process of step 1) the AAO template are as follows:
A, at least 99.99% high-purity aluminium flake is placed in tube furnace, and under nitrogen protection, 450~550 DEG C of annealing are 3~4 small
When, to remove surface stress；
B, it is cleaned by ultrasonic 4~6 minutes with acetone and alcohol, removes surface and oil contaminant；
C, using H4ClO4It in electric current is 0.5~0.7A aluminium flake with ethyl alcohol, the polishing fluid that volume ratio is 1:8~1:10
Under the conditions of, polish 1.5~2.5min；
It d, in voltage is 35~45V, the item that temperature is 9~11 DEG C aluminium flake using the oxalic acid solution of 0.3~0.5mol/L
Under part, 3.5~4.5h is aoxidized；
E, the step d aluminium flake aoxidized is placed in phosphoric acid chromic acid solution, at 55~65 DEG C, 5~7h is dried, except deoxidation
Change film；
F, using the oxalic acid solution of 0.3~0.5mol/L, aluminium flake under conditions of voltage is 35~45V, oxidation 9~
11h；
G, it dries, for use.
Preferably, the cleaning of the step 2) is cleaned with 0.8~1mol/L diluted sodium hydroxide solution, is then removed
Surface impurity keeps surfacing clean.
Preferably, AAO template is first cropped the aluminium flake part on periphery by the step 3) before electroless deposition, it is only remaining in
Between aluminium oxide, prepared solution of ferrous chloride is put into reaction kettle, AAO template is put into the mold of polytetrafluoroethylene (PTFE),
Teflon mould is wound with strike-through band and is sealed, and vacuum oven drying, the heating rate of vacuum oven are put into after deposition
It is 5~7 DEG C/min, set temperature is 140~160 DEG C, keeps the temperature 1.5~2.5h.
Preferably, gold is deposited in the step 4) in AAO template specifically comprises the processes of: by iron nanometer rods made from step 3)
The AAO template of array is placed in ion vacuum plated film instrument, the high-purity gold target that evaporation source is at least 99.999%, and vacuum degree is
3~5 × 10-6Pa, rate are 0.18~0.22A/S, and 270~330s is deposited, obtains strawberry-like Au nanosphere array substrate.
Have that preparation is simple compared with the prior art, the advantages of the present invention are as follows: the present invention, synthesis process is high
Succinct, pollution-free and at low cost feature is imitated, large area is regular, ties using being formed on Fe nanowire during vapor deposition
Structure is controllable, high sensitivity, the self assembly Au nanosphere array structure of the strawberry-like formd, the SERS substrate energy of this self assembly
The nano-array for forming coarse surface and marshalling has very high Raman enhancing activity, can reuse, improve SERS's
Stability can be widely applied in trace detection.
Detailed description of the invention
Fig. 1 is the preparation process schematic diagram of self assembly SRES substrate provided by the invention；
Fig. 2 is the shape appearance figure for the AAO template that the embodiment of the present invention 1 is prepared；
Fig. 3 a is the SEM shape appearance figure of the AAO template after growing Fe nanowire in the embodiment of the present invention 1；
Fig. 3 b is the SEM shape appearance figure of the AAO template after growing Fe nanowire in the embodiment of the present invention 2；
Fig. 3 c is the SEM shape appearance figure of the AAO template after growing Fe nanowire in the embodiment of the present invention 3；
Fig. 4 a is the shape appearance figure that the Au nano-array after gold is deposited in the embodiment of the present invention 1；
Fig. 4 b is the enlarged drawing of Au nanosphere in Fig. 4 a；
Fig. 5 a is the EDX figure of Fe nano-array in the embodiment of the present invention 1；
Fig. 5 b is the EDX figure of Au nanometers of ball arrays in the embodiment of the present invention 1；
Fig. 6 is the Raman data figure with vapor deposition gold that gold is not deposited in the embodiment of the present invention 1；
Fig. 7 is the Raman data figure before cleaning in the embodiment of the present invention 1 and after cleaning.
Specific embodiment
The present invention will be described in further detail below with reference to the embodiments of the drawings.
Embodiment 1:
A kind of method of iron nano-dot matrix auxiliary preparation self assembly strawberry-like gold SRES substrate, the specific steps are as follows:
1) the AAO template preparation of aperture 60-80nm:
A, 99.99% high-purity aluminium flake is placed in tube furnace, under nitrogen protection, 500 DEG C of 4 hours of annealing, to remove table
Face stress；
B, it is cleaned by ultrasonic 5 minutes with acetone and alcohol, removes surface and oil contaminant；
C, using H4ClO4It is thrown aluminium flake under conditions of electric current is 0.6A with the polishing fluid of ethyl alcohol (volume ratio 1:9)
Light 2min；
It d, in voltage is that 40V aoxidizes 4h under conditions of temperature is 10 DEG C aluminium flake using the oxalic acid solution of 0.4mol/L；
E, the step d aluminium flake aoxidized is placed in phosphoric acid chromic acid solution, at 60 DEG C, 6h is dried, to remove oxidation film；It adopts
10h is aoxidized aluminium flake under conditions of voltage is 40V with the oxalic acid solution of 0.4mol/L；
F, it dries, for use；The AAO template of preparation is as shown in Figure 2；60~80nm of aperture is prepared by anodizing
AAO template；
2) step 1) AAO template obtained is cleaned with 0.8~1mol/L diluted sodium hydroxide solution, removal surface is miscellaneous
Matter keeps surfacing clean；
3) the electroless deposition Fe nanowire in AAO template:
A, AAO template is cropped to the aluminium flake part on periphery, is only left intermediate aluminium oxide；
B, the Iron dichloride tetrahydrate solution of 1mol/L is prepared, measurement 35ml is put into AAO template in 50ml reaction kettle and puts into
In the mold of polytetrafluoroethylene (PTFE), Teflon mould is wound with strike-through band and is sealed；
C, setting the heating rate of stove as 6 degree of set temperatures per minute is 150 DEG C, keeps the temperature two hours；
D, it is cleaned by ultrasonic after natural cooling, drying is stand-by；
4) gold is deposited in AAO template:
The AAO template of Fe nanowire is placed in ion vacuum plated film instrument, the high-purity gold that evaporation source is 99.999%
Target, vacuum degree are 4 × 10-6Pa, rate 0.2A/S are deposited 300s, obtain the good substrate of pattern, iron nano-array is in SEM
Under pattern it is as shown in Figure 3a；The pattern of Au nanometers of ball arrays in the secure execution mode (sem is as shown in Fig. 4 a, Fig. 4 b.
Embodiment 2:
A kind of method of iron nano-dot matrix auxiliary preparation self assembly strawberry-like gold SRES substrate, the specific steps are as follows:
1) the AAO template preparation of aperture 60-80nm:
A, 99.99% high-purity aluminium flake is placed in tube furnace, under nitrogen protection, 450 DEG C of 4 hours of annealing, to remove table
Face stress；
B, it is cleaned by ultrasonic 6 minutes with acetone and alcohol, removes surface and oil contaminant；
C, using H4ClO4It is thrown aluminium flake under conditions of electric current is 0.5A with the polishing fluid of ethyl alcohol (volume ratio 1:8)
Light 2.5min；
It d, in voltage is 45V aluminium flake using the oxalic acid solution of 0.5mol/L, under conditions of temperature is 11 DEG C, oxidation
3.5h；
E, the step d aluminium flake aoxidized is placed in phosphoric acid chromic acid solution, at 65 DEG C, 5h is dried, to remove oxidation film；
F, 11h is aoxidized aluminium flake under conditions of voltage is 45V using the oxalic acid solution of 0.5mol/L；
G, it dries, for use；The AAO template of 60~80nm of aperture is prepared by anodizing；
2) step 1) AAO template obtained is cleaned with 0.8~1mol/L diluted sodium hydroxide solution, removal surface is miscellaneous
Matter keeps surfacing clean；
3) the electroless deposition Fe nanowire in AAO template:
A, AAO template is cropped to the aluminium flake part on periphery, is only left intermediate aluminium oxide；
B, the Iron dichloride tetrahydrate solution of 0.9mol/L is prepared, measurement 35ml is put into AAO template in 50ml reaction kettle and puts
Into in the mold of polytetrafluoroethylene (PTFE), Teflon mould is wound with strike-through band and is sealed；
C, set the heating rate of stove as 7 DEG C/per minute, set temperature is 160 DEG C, keeps the temperature 1.5 hours；
D, it is cleaned by ultrasonic after natural cooling, drying is stand-by；
4) gold is deposited in AAO template:
The AAO template of Fe nanowire is placed in ion vacuum plated film instrument, the high-purity gold that evaporation source is 99.999%
Target, vacuum degree are 5 × 10-6Pa, rate 0.22A/S are deposited 270s, obtain the good substrate of pattern, iron nano-array is in SEM
Under pattern it is as shown in Figure 3b.
Embodiment 3:
A kind of method of iron nano-dot matrix auxiliary preparation self assembly strawberry-like gold SRES substrate, the specific steps are as follows:
1) the AAO template preparation of aperture 60-80nm:
A, 99.99% high-purity aluminium flake is placed in tube furnace, under nitrogen protection, 550 DEG C of 3 hours of annealing, to remove table
Face stress；
B, it is cleaned by ultrasonic 4 minutes with acetone and alcohol, removes surface and oil contaminant；
C, using H4ClO4It is thrown aluminium flake under conditions of electric current is 0.7A with the polishing fluid of ethyl alcohol (volume ratio 1:10)
Light 1.5min；
It d, in voltage is 50V aluminium flake using the oxalic acid solution of 0.3mol/L, under conditions of temperature is 9 DEG C, oxidation
4.5h；
E, the step d aluminium flake aoxidized is placed in phosphoric acid chromic acid solution, at 55 DEG C, 7h is dried, to remove oxidation film；
F, 9h is aoxidized aluminium flake under conditions of voltage is 50V using the oxalic acid solution of 0.3mol/L；
G drying, for use；The AAO template of 60~80nm of aperture is prepared by anodizing；
2) step 1) AAO template obtained is cleaned with 0.8~1mol/L diluted sodium hydroxide solution, removal surface is miscellaneous
Matter keeps surfacing clean；
3) the electroless deposition Fe nanowire in AAO template:
A, AAO template is cropped to the aluminium flake part on periphery, is only left intermediate aluminium oxide；
B, the Iron dichloride tetrahydrate solution of 1.2mol/L is prepared, measurement 35ml is put into AAO template in 50ml reaction kettle and puts
Into in the mold of polytetrafluoroethylene (PTFE), Teflon mould is wound with strike-through band and is sealed；
C, set the heating rate of stove as 5 DEG C/per minute, set temperature is 140 DEG C, keeps the temperature 2.5 hours；
D, it is cleaned by ultrasonic after natural cooling, drying is stand-by；
4) gold is deposited in AAO template:
The AAO template of Fe nanowire is placed in ion vacuum plated film instrument, the high-purity gold that evaporation source is 99.999%
Target, vacuum degree are 3 × 10-6Pa, rate 0.18A/S are deposited 330s, obtain the good substrate iron nano-array of pattern in SEM
Under pattern it is as shown in Figure 3c.
Steps are as follows for performance test:
1) Raman enhancing test is done with the R6G of various concentration:
A, rhodamine R6G is configured to the solution (10 of various concentration-4, 10-6, 10-8, 10-10With 10-12mol/L)；
B, the substrate after will be gold-plated is protected from light in various concentration rhodamine R6G respectively impregnates 4h；
C, the laser of 50X mirror and 532nm wavelength is selected to do Raman test；
2) substrate for doing test is cleaned, the Raman that tries again test:
A, substrate is impregnated in acetone, is cleaned by ultrasonic 5min, then rinsed with deionized water；
B, substrate is immersed in dehydrated alcohol, continues to be cleaned by ultrasonic 5min；Natural air drying after the completion, for use；
C, by the substrate after cleaning 10-4It is protected from light in mol/L rhodamine R6G solution and impregnates 4h；
D, the laser of 50X mirror and 532nm wavelength is selected to do Raman test again.
The Raman test result of embodiment 1 is as shown in Figures 6 and 7, the Raman test result and 1 class of embodiment of embodiment 2 and 3
Seemingly.
By Fig. 1~7 it can be seen that
Fig. 1 is the 3D schematic diagram of the preparation process of SRES substrate, and AAO template by electroless deposition, receive by the long tapping in hole
Then rice noodles form uniform self assembly Au nanometers of ball arrays on iron nano-array surface using Vacuum Coating method.
As shown in Fig. 2, the AAO template of two step anodic oxidations forms a large amount of sequential holes arrays, the upper surface in each hole
There are 6 protrusions at edge, forms 6 vertex of hexagon, and hole is evenly distributed in six corner apertures, furthermore, it is possible to from figure 2, it is seen that
The size in aperture is 60~80nm.
In addition, the time span of oxidation, oxidation solution concentration and type, the voltage of oxidation will affect pore size.Therefore, have
Necessity selects suitable concentration and voltage according to the needs in aperture.As shown in figure 3, after electroless deposition, shape in AAO template
At the nano-wire array of marshalling, Fig. 3 a, b, c are obtained after changing oxidation voltage reaction temperature in embodiment 1,2,3 respectively
The electron microscope of the nano wire arrived, it is evident that can see that the diameter of nano wire changes with the variation of voltage and oxidization time.Cause
This, by change AAO template nanoporous size can obtain the nano wire with different-diameter, thus between nano wire between
Away from also changing therewith.As shown in Figure 5 a, which indicates other than Al and O for the EDX analysis of Fe nano-array, and there are Fe members
Element, this shows that the composition of nano wire is Fe, and the peak Al and O belongs to aluminium foil and Cl element is from FeCl2, during the deposition process, Fe2+
Ion obtains electronics and is simultaneously reduced into Fe on the surface Al, and then, over time, nano wire is formed, this process can be with
It is considered as a kind of galvanic interaction, wherein Al is oxidized to Al3+And Fe2+It is reduced into Fe.
As shown in fig. 4 a, after the AAO template of long nanowire being steamed gold, Au nanometers of ball array of uniform size is formd；
In fig. 4b, Au nanometers of ball surfaces have been covered with smaller nanosphere, and whole is in strawberry-like, so as to form coarse table
Face；The diameter of nanosphere is in 100nm or so.As shown in Figure 5 b, the peak Al and O belongs to aluminium foil, Au table for the EDX analysis of Au nano-array
The composition of bright nano-array is exactly gold.
As shown in fig. 6, selecting the rhodamine (rhodamine 6G, R6G) of various concentration to be used as probe, to arranged in a uniform
Au nano-dot matrix carries out surface Raman enhancement test.When sample measures, using laser capture microdissection Raman spectrometer, 50X long away from
Object lens, time of integration 1s, integral number of times 3, excitation wavelength 532nm.Fig. 6 be concentration rhodamine (rhodamine 6G,
R6G) in the Raman spectrum of Au nano-dot matrix substrate, using R6G as probe molecule, the curve of spectrum under various concentration, with rhodamine institute
Corresponding concentration is (a) 10-4mol/L；(b)10-6mol/L；(c)10-8mol/L；(d)10-10mol/L；(e)10-12mol/L.From
Fig. 6 can be seen that when rhodamine (rhodamine 6G, R6G) concentration is gradually increased, and the diffraction maximum of Raman spectrum adds therewith
By force, with 599,763,1173,1298 and 1351,1498,1637cm-1The diffraction maximum at place represents the characteristic peak of R6G, rhodamine
(rhodamine 6G, R6G) concentration is 10-4Mol/L reinforcing effect is most obvious；Rhodamine (rhodamine 6G, R6G) concentration is
10-12When mol/L, 599,763,1173,1298 and 1351,1498,1637cm-1Still there is faint peak at place.In the upper left Fig. 6
In the figure of angle as can be seen that in 1637cm-1The diffraction maximum at place enhances as the concentration of R6G increases.In conjunction with SEM map analysis, substrate
Upper gold nanosphere is large number of, and ball surface has a large amount of smaller size of nanosphere, so as to form between more nanometers
Gap, it is also more than common nanosphere permutation that Raman enhances " hot spot ", therefore couples enhancing and also reinforced, thus substrate energy
Detect 10-12Rhodamine (rhodamine 6G, R6G), reinforcing effect has reached 1012Times or more.
As shown in fig. 7, there are the Raman signals of Au nano-dot matrix diffraction maximum occurs, it is able to detect R6G (curve a).Separately
Outside, by the Au nano-dot matrix after cleaning, in the same area acquisition SERS signal, (curve b), test specification Au nano-dot matrix can be weighed
It is multiple to use.Not having R6G, without the AAO template of Au nano-dot matrix, (curve d) does not have diffraction maximum yet.This cleaning process is included in acetone
Middle ultrasonic treatment 60 seconds, is immersed in alcohol, and rinse in deionized water, then dry in surrounding air.After cleaning
There is weaker diffraction maximum in Au nano-dot matrix, this can should solve (curve c) by being repeated several times to clean.
In conclusion the present invention has preparation process simple, synthesis process is efficient, pollution-free, feature at low cost: a side
Face, present invention process is simple, and not needing cumbersome procedure of processing, (such as complicated oxygen rie, ion beam etching, atom steam
Plating method, the processing technologys such as sol-gal process), also eliminate high-cost instrument；On the other hand, strawberry-like Au nano-array can be certainly
Assembling is formed, and is not needed extraly to regulate and control micro-nano structure, is saved a large amount of time and energy.This large area rule
Orderly, structure-controllable, high sensitivity strawberry-like Au nanosphere array structure as SERS substrate when, coarse surface can be formed
With the array of marshalling, thus there is very high Raman enhancing activity, and can reuse, with preferable stability,
It can be widely applied in trace detection.
Claims (5)
1. a kind of method of iron nano-dot matrix auxiliary preparation self assembly strawberry-like gold SRES substrate, it is characterised in that including following step
It is rapid:
1) the AAO template of 60~80nm of aperture is prepared by anodizing；
2) the AAO template by step 1) preparation cleans impurity elimination, keeps surfacing clean；
3) the electroless deposition Fe nanowire in AAO template: 0.9~1.2mol/L solution of ferrous chloride is prepared, electroless deposition is passed through
Iron nanometer rods grow it according to the aperture of AAO template；It is dry that it is put into vacuum oven after deposition, obtains regular array
Iron nanometer stick array；
4) gold is deposited in AAO template: using Vacuum Coating method, it is obtained that gold particle is plated in step 3) in the environment of vacuum
In the AAO template of iron nanometer stick array, the substrate with Au nanometers of ball arrays of strawberry-like is obtained.
2. according to the method described in claim 1, it is characterized by: the specific preparation process of step 1) the AAO template are as follows:
A, at least 99.99% high-purity aluminium flake is placed in tube furnace, under nitrogen protection, 450~550 DEG C of 3~4 hours of annealing,
To remove surface stress；
B, it is cleaned by ultrasonic 4~6 minutes with acetone and alcohol, removes surface and oil contaminant；
C, using H4ClO4It is the polishing fluid of 1:8~1:10 with ethyl alcohol, volume ratio, aluminium flake in the condition that electric current is 0.5~0.7A
Under, polish 1.5~2.5min；
It d, in voltage is 35~45V, the condition that temperature is 9~11 DEG C aluminium flake using the oxalic acid solution of 0.3~0.5mol/L
Under, aoxidize 3.5~4.5h；
E, the step d aluminium flake aoxidized is placed in phosphoric acid chromic acid solution, at 55~65 DEG C, dries 5~7h, to remove deoxidation
Film；
F, 9~11h is aoxidized aluminium flake under conditions of voltage is 35~45V using the oxalic acid solution of 0.3~0.5mol/L；
G, it dries, for use.
3. according to the method described in claim 1, it is characterized by: the cleaning of the step 2) is with the dilute hydrogen of 0.8~1mol/L
Sodium hydroxide solution is cleaned, and surface impurity is then removed, and keeps surfacing clean.
4. according to the method described in claim 1, it is characterized by: the step 3) first cuts out AAO template before electroless deposition
The aluminium flake part on periphery is cut, is only left intermediate aluminium oxide, prepared solution of ferrous chloride is put into reaction kettle, AAO
Template is put into the mold of polytetrafluoroethylene (PTFE), and Teflon mould is wound with strike-through band and sealed, and is put into vacuum drying after deposition
Case is dry, and the heating rate of vacuum oven is 5~7 DEG C/min, and set temperature is 140~160 DEG C, keeps the temperature 1.5~2.5h.
5. according to the method described in claim 1, it is characterized by: the specific work of gold is deposited in the step 4) in AAO template
Skill are as follows: the AAO template of iron nanometer stick array made from step 3) is placed in ion vacuum plated film instrument, evaporation source is at least
99.999% high-purity gold target, vacuum degree are 3~5 × 10-6Pa, rate are 0.18~0.22A/S, and 270~330s is deposited, obtains
To strawberry-like Au nanosphere array substrate.
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