CN105112913B - A kind of transferable Fe2O3/ Au nano-pore array thin films and preparation method thereof - Google Patents
A kind of transferable Fe2O3/ Au nano-pore array thin films and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to technical field of nano material, and in particular to a kind of transferable Fe2O3/ Au nano-pore array thin films and preparation method thereof.The film that the present invention is provided is by Au nano-pore array thin films and is overlying on Fe thereon2O3Nano-pore array thin film is constituted, the nano-pore up/down perforation in double-layer filmses, is arranged by the Hexagonal Close-packed order of rule.The preparation method of the film is as follows:Porous alumina formwork is chosen, Au films are sputtered on a surface of template, then using electro-deposition method in one layer of Fe nano-pore array thin film of Au nano-pore array thin films superficial growth, next Low Temperature Heat Treatment makes Fe be converted into Fe in atmosphere2O3, target product is finally made after alumina formwork using except coating solution is removed.The inventive method is simple and convenient to operate, cost is low, and gained membrane pore size is controllable, aligned orderly, film are transferable, can be applied to electrochemical sensor and biology sensor, can obtain sensitive stablizing believable response signal.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of transferable Fe2O3/ Au nano-pore array thin films
And preparation method thereof.
Background technology
Fe2O3As the oxide of most stable of iron under normal temperature, with cheap, abundant raw material, environment-friendly, improved corrosion
The advantages of property, it can be applied to pigment, gas sensor, catalyst and various hard and soft magnetic materials.Nanometer Fe2O3Relative to tradition
Fe2O3Performance has significant increase for material, is increasingly becoming the study hotspot of related device material.But with science
The progress of technology, to nanometer Fe2O3Research is also on the increase, structured size uniform nanometer special to exploitation pattern
Fe2O3Tighter higher target be it is also proposed, it is necessary to constantly improve and improve existing method or develop new excellent performance
Fe2O3Nano material and preparation method thereof.
Nanometer Fe2O3With good catalytic activity and bio-compatibility, therefore on electrochemical sensing and bio-sensing
Using increasingly being paid close attention to by people.In recent years, based on nanometer Fe2O3The electrochemical sensing device and biology sensor of material
Part is constantly reported.But usual prepared α types Fe2O3The electric conductivity of nano material is poor, and electron mobility is relatively low,
This seriously constrains the activity of its catalytic reaction, have impact on the performance of respective sensor part.Research shows that Au nanostructureds are not only
It with good electric conductivity, and can also stablize and rapidly adsorbed proteins, and keep its bioactivity, accelerate protein
Electro transfer between electrode.Therefore in order to improve Fe2O3The electric conductivity of nano material, if it is possible to by Fe2O3Constituted with Au
Composite nanostructure, is undoubtedly possible to greatly promote the detection performance of respective sensor part.
In addition, Fe2O3The preparation of nano material is prepared frequently with hydro-thermal method, sol-gal process, high-temperature decomposition etc.
Nano material often due to specific surface area big in high temperature crystallization process and cause surface-active higher, easily form high degree of agglomeration
Nanoclusters structure, will also have a strong impact on the performance of respective sensor.And nano-pore array thin film has well-regulated pore structure,
Nano material can be made while large specific surface area is kept and high surfaces are active, it is to avoid the reunion between material, it is received
Meter level pore space structure can also promote the absorption of solution and the transmission of ion, can be dropped significantly in terms of electrochemical analysis and bio-sensing
Low signal-to-noise ratio, improves sensitivity, accelerates response speed etc., therefore with very high use value.But at present, do not have been reported that also and adopt
Use Fe2O3Nano-pore array thin film or Fe2O3Electrochemical sensing or the function of bio-sensing prepared by/Au nano-pore array thin films
Device.
The content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art there is provided a kind of transferable Fe2O3/ Au nanohole arrays are thin
Film.
The technical scheme is that a kind of transferable Fe2O3/ Au nano-pore array thin films are thin by Au nanohole arrays
Film and it is overlying on Fe thereon2O3Nano-pore array thin film is constituted, the nano-pore up/down perforation in double-layer filmses, by the hexagonal of rule
Solid matter order is arranged, and the diameter in the hole is 10~50nm, and pitch of holes is 100~120nm, and the gross thickness of the film is
60~150nm.
Present invention also offers Fe2O3The preparation method of/Au nano-pore array thin films, comprises the following steps:
Step 1, porous alumina formwork is chosen, Au films are sputtered on a surface of template, concrete operations are as follows:Porous
Alumina formwork is placed in magnetron sputtering or ion sputtering, and target used is gold target, on a surface of porous alumina formwork
Sputtering last layer thickness is the continuous Au films that 30~70nm has nano aperture, as working electrode during electrochemical deposition, with
And the base layer and conductive layer of final goal product;
Step 2, the porous alumina formwork of above-mentioned sputtering Au films is put into the electrolytic iron liquid in electrolytic cell, wherein there is Au
The one of film is facing to solution, and another side sealing makes it not contacted with solution, then using graphite as to electrode, in current density 0.6~
1.2mA/cm2Lower use two-probe method electro-deposition 5~15 minutes, obtains the nano-pore array thin film of metallic iron;
Step 3, the alumina formwork that there are Fe/Au nano-porous thin films will be grown to be placed in Muffle furnace, sets that temperature is constant to be
150~200 DEG C, keep the temperature after 2~4 hours under the atmosphere of air, naturally cool to room temperature, by Fe nano-porous thin films heat
It is oxidized to Fe2O3Nano-porous thin film, is finally made target product using except coating solution is removed after alumina formwork.
It is preferred that, selected porous alumina formwork aperture is 40~80nm in step 1, pitch of holes is 100~
120nm。
It is preferred that, purity >=99.999% of gold target described in step 1.
Specifically, in step 2 electrolytic iron liquid by 160g/L ferrous sulfate, 60g/L ammonium sulfate, 3.5g/L Vitamin C
The boric acid of acid, 2ml/L glycerine and 14.3g/L is mixed, and described concentration is mixed ultimate density.
Specifically, the NaOH solution that coating solution is 2mol/L of removing described in step 3.
In the present invention, nano-pore array thin film is preferably the Hexagonal array of rule, is easy to make target product more neatly draw
One, so as to improve the repeatability of preparation, corresponding material property is also more stablized.Electrolytic iron liquid is preferably that 160g/L sulfuric acid is sub-
Iron, 60g/L ammonium sulfate, 3.5g/L ascorbic acid, 2ml/L glycerine and 14.3g/L boric acid are mixed, and are not only
Obtained target product is laid a good foundation, and also makes electro-deposition easy to implement.
Beneficial effects of the present invention:
The Fe of the present invention2O3/ Au nano-pore array thin films had both maintained the major advantage of continuous film, while it is orderly
Loose structure can greatly increase the specific surface area of film again, sensitivity when being conducive to improving electrochemical analysis.Nanohole array
Film uses orderly Hexagonal array, is easy to make target product more uniform, so that the repeatability of preparation is improved, corresponding material
Expect that performance is also more stablized.Second, obtained Fe2O3/ Au nano-pore array thin films have good transferability (such as Fig. 2 institutes
Show, the film after preparing can be in floating on water, after being fished for required substrate from water, drying), it is transferred to any
The substrate that even bends of substrate on, this causes film can be carried out in nonconducting substrate or on the substrate of bending
Effective application.Third, to obtained Fe2O3/ Au nano-pore array thin films are transferred on ito glass substrate and by edge with having
After the sealing of machine glue, the fast electrochemical that can be directly used in ascorbic acid is determined, and utilizes Fe2O3Obtained by/Au nano-pore array thin films
Sensor electrode have the advantages that the response time is short, test limit is low, sensitivity is high, stability is good, cost is low, and resist
The detection efficiency of bad hematic acid is high, and the degree of accuracy is high.Fourth, the technique of preparation method of the present invention is simple, cost is relatively low, production efficiency
Height, suitable for large-scale production, can also promote the nano-pore array thin film for synthesizing other materials combination.
Brief description of the drawings
Fig. 1 is Fe2O3The schematic diagram of/Au nano-pore array thin film preparation flows.
Fig. 2 is on different substrates by Fe2O3/ Au nano-pore array thin films carry out the photo of transfer operation, wherein figure a institutes
Transfer method is shown as, the film floating that will specifically prepare stretches into water on the water surface with required substrate (being ito glass in figure)
In, gently fished for from film lower section, then dry or dry.Figure b is the design sketch that film is transferred on ito glass.Scheme c
The design sketch in the ITO/ polyester substrates of flexibility is transferred to for film.Figure d is the effect on the glass bar surface that film is transferred to circle
Fruit is schemed.
Fig. 3 is the knot that target product made from case study on implementation 1 uses field emission scanning electron microscope (SEM) to be characterized
Really;Wherein, Fig. 3 b are the oblique views of target product.
Fig. 4 is the result that target product made from case study on implementation 1 uses X-ray diffractometer (XRD) to be characterized, abscissa
For angle of diffraction, ordinate is diffracted intensity.
Fig. 5 is with Fe made from case study on implementation 12O3/ Au nano-pore array thin films are resisted as without enzyme electrochemical sensing electrode
Bad hematic acid (AA) detect obtained chronoa mperometric plot, and the AA of 1mM concentration meter is continuously added to when wherein left figure is detection
When current-responsive figure, right figure for detection when add corresponding chrono-amperometric response diagram after small concentration AA, two figures show thin-film electro
Has performance that is sensitive, stably, quickly detecting AA.Left figure shows current-responsive fast and stable during detection, and right figure shows inspection
Current-responsive is sensitive quick during survey.
Fig. 6 (a) and (b) be respectively case study on implementation 2 and 3 made from target product use field emission scanning electron microscope
(SEM) result characterized, it can be seen that the corresponding film average pore sizes of Fig. 6 a are 30nm, the corresponding film average pore sizes of Fig. 6 b
It is 10nm.
Embodiment
Raw materials market used in following embodiments is bought or is made with conventional method:
Aperture is 40~80nm, and pitch of holes is 100~120nm porous alumina formwork;By 160g/L ferrous sulfate,
The electrolytic iron that 60g/L ammonium sulfate, 3.5g/L ascorbic acid, 2ml/L glycerine and 14.3g/L boric acid are mixed
Liquid;2mol/L NaOH solution;The Au targets of purity >=99.999%.
Embodiment 1 prepares Fe2O3/ Au nano-pore array thin films
Step 1, it is 80nm to choose aperture, and pitch of holes is 120nm porous alumina formwork, is splashed on a surface of template
Au films are penetrated, method is that porous alumina formwork is placed in ion sputtering, target used is gold target, in porous alumina formwork
One surface sputtering last layer thickness is the continuous Au films that 30nm has nano aperture, is used as work electricity during electrochemical deposition
Pole, and final goal product base layer and conductive layer;
Step 2, the porous alumina formwork of above-mentioned sputtering Au films is put into the electrolytic iron liquid in electrolytic cell, wherein there is Au
The one of film is facing to solution, and another side sealing makes it not contacted with solution, then using graphite as to electrode, in current density
0.8mA/cm2Lower use two-probe method electro-deposition 10 minutes, obtains the nano-pore array thin film of metallic iron;
Step 3, the alumina formwork that there are Fe/Au nano-porous thin films will be grown to be placed in Muffle furnace, sets that temperature is constant to be
150 DEG C, keep the temperature after 3 hours under the atmosphere of air, naturally cool to room temperature, be by Fe nano-porous thin film thermal oxides
Fe2O3Nano-porous thin film, finally removes in 2mol/L NaOH solution and target product, preparation flow is made after alumina formwork
Schematic diagram it is as shown in Figure 1.
In aqueous by the Fe prepared2O3/ Au nano-pore array thin films are transferred to ito glass, polyester plastics, glass
Photo on glass rod can be protected in transfer process as shown in Fig. 2 show that prepared film has good transferability
Hold preferable continuity and integrality.
Obtained target product is characterized using field emission scanning electron microscope (SEM), acquired results such as Fig. 3 a
It is shown.Prepared Fe it can be seen from SEM photograph2O3/ Au nano-pore array thin films are in interior aligned orderly in a big way, often
Uniform solid matter 6 holes around individual hole, and pore size is uniform, in irregular circular configuration, and the size in hole is 50nm, is slightly less than
The aperture of porous alumina formwork, the gross thickness of film is tested to be 100nm.Each can be seen that by the oblique view 3b of amplification
Hole is 50nm or so particle all around the particle diameter of six symmetric arrays, and these particles are closely joined together, overall
Fairly regular arrangement is showed, this regular contoured surface causes prepared Fe2O3/ Au nano-pore array thin films have
Very big specific surface area, can substantially reduce signal to noise ratio in terms of electrochemical analysis and bio-sensing, improve sensitivity, accelerate response
Speed etc..
Obtained target product is characterized using X-ray diffractometer (XRD), acquired results are as shown in Figure 4.From spectrogram
In as can be seen that target product by Fe2O3With Au compositions, understand that product is Fe with reference to preparation process2O3/ Au array films.
By Fe2O3/ Au nano-pore array thin films be transferred on ito glass substrate and seal at edge with organic gel after as
Working electrode, platinum electrode is that, to electrode, Ag/AgCl electrodes are reference electrode, constitute three-electrode system;, will during electrochemical gaging
The electrode is placed in the 0.2mol/L stirred with constant rate of speed NaOH solution;Then one is applied on the working electrode (s constant
Current potential (0.6V), record current-time curvel, after background current reaches stable state, with microsyringe add various concentrations
Ascorbic acid solution sample, and record current responds, corresponding timing during the corresponding ascorbic acid solution concentration of obtained addition
Results of weak current is as shown in Figure 5, it can be seen that the change in concentration of sensor Ascorbic Acid has the response of rapid sensitive, during response
Between be less than 5 seconds, when being continuously added to same concentrations ascorbic acid, corresponding curent change is in the same size and stably, can be calculated
Sensitivity reaches 1262 μ A/mMcm2, test limit can as little as 1 μm ol/L, show Fe2O3The confrontation of/Au nano-pore array thin films is bad
The oxidation of hematic acid has good catalytic capability.
Embodiment 2 prepares Fe2O3/ Au nano-pore array thin films
Step 1, it is 40nm to choose aperture, and pitch of holes is 100nm porous alumina formwork, is splashed on a surface of template
Au films are penetrated, method is that porous alumina formwork is placed in ion sputtering, target used is gold target, in porous alumina formwork
Surface sputtering last layer thickness be continuous Au films that 40nm has nano aperture, be used as work electricity during electrochemical deposition
Pole, and final goal product base layer and conductive layer;
Step 2, the porous alumina formwork of above-mentioned sputtering Au films is put into the electrolytic iron liquid in electrolytic cell, wherein there is Au
The one of film is facing to solution, and another side sealing makes it not contacted with solution, then using graphite as to electrode, in current density
0.6mA/cm2Lower use two-probe method electro-deposition 5 minutes, obtains the nano-pore array thin film of metallic iron;
Step 3, the alumina formwork that there are Fe/Au nano-porous thin films will be grown to be placed in Muffle furnace, sets that temperature is constant to be
150 DEG C, keep the temperature after 2 hours under the atmosphere of air, naturally cool to room temperature, be by Fe nano-porous thin film thermal oxides
Fe2O3Nano-porous thin film, finally removes in 2mol/L NaOH solution and target product, preparation flow is made after alumina formwork
Schematic diagram as shown in figure 1, products therefrom Fe2O3The stereoscan photograph of/Au nano-pore array thin films as shown in Figure 6 a, its XRD
Test and Electrochemical results are similar with Fig. 4 and Fig. 5.
Embodiment 3 prepares Fe2O3/ Au nano-pore array thin films
Step 1, it is 60nm to choose aperture, and pitch of holes is 100nm porous alumina formwork, is splashed on a surface of template
Au films are penetrated, method is that porous alumina formwork is placed in ion sputtering, target used is gold target, in porous alumina formwork
One surface sputtering last layer thickness is the continuous Au films that 70nm has nano aperture, is used as work electricity during electrochemical deposition
Pole, and final goal product base layer and conductive layer;
Step 2, the porous alumina formwork of above-mentioned sputtering Au films is put into the electrolytic iron liquid in electrolytic cell, wherein there is Au
The one of film is facing to solution, and another side sealing makes it not contacted with solution, then using graphite as to electrode, in current density
1.2mA/cm2Lower use two-probe method electro-deposition 15 minutes, obtains the nano-pore array thin film of metallic iron;
Step 3, the alumina formwork that there are Fe/Au nano-porous thin films will be grown to be placed in Muffle furnace, sets that temperature is constant to be
200 DEG C, keep the temperature after 4 hours under the atmosphere of air, naturally cool to room temperature, be by Fe nano-porous thin film thermal oxides
Fe2O3Nano-porous thin film, finally removes in 2mol/L NaOH solution and target product, preparation flow is made after alumina formwork
Schematic diagram as shown in figure 1, products therefrom Fe2O3The stereoscan photograph of/Au nano-pore array thin films as shown in Figure 6 b, its XRD
Test and Electrochemical results are similar with Fig. 4 and Fig. 5.
Although the present invention is disclosed as above with preferred embodiment, and the non-limiting present invention, any those skilled in the art
Member without departing from the spirit and scope of the present invention, can be suitably modified.Therefore, the scope of the present invention is with claim institute circle
Fixed scope is defined.
Claims (6)
1. a kind of transferable Fe2O3/ Au nano-pore array thin films, it is characterised in that:By Au nano-pore array thin films and being overlying on it
On Fe2O3Nano-pore array thin film is constituted, the nano-pore up/down perforation in double-layer filmses, is arranged by the Hexagonal Close-packed order of rule
Row, the diameter in the hole is 10~50nm, and pitch of holes is 100~120nm, and the gross thickness of the film is 60~150nm.
2. Fe described in claim 12O3The preparation method of/Au nano-pore array thin films, it is characterised in that:Comprise the following steps:
Step 1, porous alumina formwork is chosen, Au films are sputtered on a surface of template, concrete operations are as follows:Porous oxidation
Aluminum alloy pattern plate is placed in magnetron sputtering or ion sputtering, and target used is gold target, is sputtered on a surface of porous alumina formwork
Last layer thickness is the continuous Au films that 30~70nm has nano aperture, as working electrode during electrochemical deposition, and most
The base layer and conductive layer of whole target product;
Step 2, the porous alumina formwork of above-mentioned sputtering Au films is put into the electrolytic iron liquid in electrolytic cell, wherein there are Au films
One facing to solution, another side sealing, it is not contacted with solution, then using graphite as to electrode, in current density 0.6~
1.2mA/cm2Lower use two-probe method electro-deposition 5~15 minutes, obtains the nano-pore array thin film of metallic iron;
Step 3, the alumina formwork that has Fe/Au nano-porous thin films will be grown to be placed in Muffle furnace, set temperature it is constant be 150~
200 DEG C, keep the temperature after 2~4 hours under the atmosphere of air, naturally cool to room temperature, by Fe nano-porous thin film thermal oxides
For Fe2O3Nano-porous thin film, is finally made target product using except coating solution is removed after alumina formwork.
3. method as claimed in claim 2, it is characterised in that:Selected porous alumina formwork aperture is 40 in step 1
~80nm, pitch of holes is 100~120nm.
4. method as claimed in claim 2 or claim 3, it is characterised in that:Purity >=99.999% of gold target described in step 1.
5. method as claimed in claim 2 or claim 3, it is characterised in that:In step 2 electrolytic iron liquid by 160g/L ferrous sulfate,
60g/ ammonium sulfate, 3.5g/L ascorbic acid, 2ml/L glycerine and 14.3g/L boric acid are mixed, described concentration
It is mixed ultimate density.
6. method as claimed in claim 2 or claim 3, it is characterised in that:The NaOH that coating solution is 2mol/L of removing described in step 3
Solution.
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CN107099817A (en) * | 2017-04-13 | 2017-08-29 | 合肥工业大学 | A kind of preparation method of doped ferric oxide nanometer line ordered array light anode |
CN107823705B (en) * | 2017-10-27 | 2020-01-17 | 山东大学 | Polylactic acid array with different nano-column diameters and preparation method and application thereof |
CN108557754B (en) * | 2018-04-13 | 2020-11-10 | 杭州电子科技大学 | Preparation method of self-supporting metal nano-pore film |
CN111289580A (en) * | 2018-06-27 | 2020-06-16 | 成都新柯力化工科技有限公司 | Film sensing material for detecting atmosphere hydrogen sulfide gas and preparation method thereof |
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