CN108178120A - The pattern of anodic alumina films surface nanometer array and controlled in nanometer confinement space its pattern grow method, application - Google Patents
The pattern of anodic alumina films surface nanometer array and controlled in nanometer confinement space its pattern grow method, application Download PDFInfo
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Abstract
The present invention provides the pattern of anodic alumina films surface nanometer array and the method for its pattern growth, application is controlled in nanometer confinement space, the pattern of the anodic alumina films surface nanometer array is made of the nano-array of pellumina and pellumina surface, the nano-array is 8 nanohole arrays of ZIF, and the nano-pore array structure is evenly distributed；The depth in hole is 60 ± 5 μm, and depth-to-width ratio is (4.7 ± 3) × 103.Anodic alumina films surface nanometer array provided by the invention studies intermolecular interaction in biophysics, biochemistry, ion detection, is catalyzed, separation, the application in the fields such as energy storage.The present invention provides the pattern of anodic alumina films surface nanometer array and the method for its pattern growth, application is controlled in nanometer confinement space, and synthetic method is simple, at low cost, and pattern is easy to observation and detection.Obtained nanometer material structure is stablized, stable in physicochemical property, and can be recycled.
Description
Technical field
The present invention relates to field of nanometer material technology, and in particular to the pattern of anodic alumina films surface nanometer array and in nanometer
Method, the application of its pattern growth are controlled in confinement space.
Background technology
The guess of nanopore DNA sequencing is proposed from the 1990s, and aperture is stablized, the good solid-state of physical and chemical performance
Nano pore becomes the research object of biophysics and biochemical research.By duct interior finishing, the solid-state after functionalization
It is big to decode biology for nano pore, the interaction between large biological molecule is studied, medical diagnosis on disease, drug delivery, ion detection
Good test performance is shown in terms of the bio-sensings such as each level structure of molecule and function.Following nano pore is in life science
Application will be widened, nano-pore technology will be the mankind life bring profound influence.
In recent years, solid nano duct method of modifying is most of by surface chemical modification, sulfydryl self-assembly method, and chemistry is heavy
The methods of area method, plasma treatment, makes inner surfaces of pores functionalization.The material of modification be biomaterial, high molecular material, your gold
Belong to the materials such as material, nano-particle.Material category and function used is relatively fewer, and the limitation of material will directly influence
The application range of nano pore.The speed of growth of the existing nano-array in duct be too fast and bad control, also can not be straight
Supervision growth course is connect, is be easy to cause after reacting under Electronic Speculum, nano particle diameter and required feature of interest difference are excessive.Therefore in hole
Other novel functional materials are successfully introduced into road, and the material is controllable in duct inside dimension, to nano-scale duct
Potential application has more important value.
Metal-organic framework materials (Metal-organic framework abbreviations MOFs, MOF) be develop nearly ten years it is fast
A kind of coordination polymer of speed has three-dimensional pore structure, is important novel more of another class except zeolite and carbon nanotube
Porous materials.So the present invention will introduce ZIF-8 materials and modify in solid nano duct, to treat excavation MOF material structures
The potential application in composite Nano duct built.
Invention content
The present invention is for the duct of modified metal organic framework material in nanometer confinement space in the prior art, nano particle
The problem of grain size and its bad control of array arrangement and complicated nano-array growth course monitoring means, it is proposed that anodised aluminium
The pattern of film surface nano-array and controlled in nanometer confinement space its pattern grow method, application.
One aspect of the present invention provides the pattern of anodic alumina films surface nanometer array, and the anodised aluminium film surface is received
The pattern of rice array is made of the nano-array of pellumina and pellumina surface, and the nano-array is ZIF-8 nanometers
Hole array, the nano-pore array structure are evenly distributed；The depth in hole is 60 ± 5 μm, and depth-to-width ratio is (4.7 ± 3) × 103。
Another aspect of the present invention offer controls above-mentioned anodic alumina films surface nanometer array in nanometer confinement space
The method of pattern growth, is as follows：
Step 1, stock, Zn (NO3)2·6H2The methanol solution of O, the methanol solution of 2-methylimidazole, the sun of different size
Pole pellumina；
Step 2, at room temperature, by Zn (NO3)2·6H2After the methanol solution mixing of the methanol solution and 2-methylimidazole of O
To the reaction solution of ZIF-8；
Step 3 after the anodic alumina films of different size are cleaned by ultrasonic 1~5min, is put into Zn (NO3)2·6H2O's
25min~35min is impregnated in methanol solution；
Step 4 takes out the anodic alumina films of soaking mistake in step 3, blots the solution of film surface, anodic oxidation
Aluminium film is passed through the ZIF-8 reaction solutions prepared in step 2 and is filtered, and ZIF-8 just starts to grow using cell walls as substrate, lasting to take out
Filter, ZIF-8 can be filled in the bulky grain of formation rule in duct gradually.Wherein, it is 50~90min to filter the time；
Above-mentioned steps one can control the size and the speed of growth of nano particle to step 4.
Further, Zn (NO in the step 13)2·6H2The methanol solution of O is by 5g Zn (NO3)2·6H2O is dissolved in
It is made in 250mL methanol.
Further, the methanol solution of 2-methylimidazole is to be dissolved in 250 mL by 2.5g 2-methylimidazoles in the step 1
It is made in methanol.
Further, the specification of the anodic alumina films is：71 ± 7.88nm, 100 ± 14.27nm, 249 ± 32.97nm
One or more of with 317 ± 36.17nm；The thickness of anodic alumina films is 60 ± 5 μm.
Further, in the step 2, Zn (NO3)2·6H2The body of the methanol solution of O and the methanol solution of 2-methylimidazole
Product is than being 1:1.
Further, soaking temperature is maintained at 50 DEG C~60 DEG C in the step 3.
Further, it is 55~60min that the time is filtered in the step 4.
Further, ZIF-8 grain diameters are 225~252nm in duct in the step 4.
The present invention also provides a kind of anodic alumina films surface nanometer arrays in biophysics, biochemistry, ion detection,
Intermolecular interaction is studied, is catalyzed, separation, the application in energy storage field.
Beneficial effects of the present invention are embodied in：
1. the present invention provides the pattern of anodic alumina films surface nanometer array and its shape is controlled in nanometer confinement space
MOF materials and solid nano duct material are combined by the method for looks growth, application, the present invention for the first time.In view of nano pore
The three dimensional topology and type of confinement effect and porous MOF (metal-organic framework materials) material it is rich, therefore by two
Kind functional material is effectively combined together.
2. the present invention provides the pattern of anodic alumina films surface nanometer array and its shape is controlled in nanometer confinement space
The method of looks growth, application, synthetic method is simple, at low cost, and pattern is easy to observation and detection.Obtained nanometer material structure is steady
It is fixed, stable in physicochemical property, and can be recycled.
The hole and size of 3.MOF porous materials are very clear and definite, it will assign solid nano duct three-dimensional topology property.And
Nano pore can give MOF materials to provide stable carrier.
4. anodic alumina films surface nanometer array provided by the invention has larger development potentiality, will be in biological object
Reason, biochemistry, ion detection study intermolecular interaction, are catalyzed, separation, and the fields such as energy storage are used widely.
Other features and advantages of the present invention will be illustrated in the following description, and partly becomes from specification
It is clear that understood by implementing the present invention.The main object of the present invention and further advantage can be by specification, power
Specifically noted scheme is realized and is obtained in sharp claim.
Description of the drawings
Fig. 1 a and Fig. 1 b are AAO fenestras road by comparison diagram before and after ZIF-8 modifications.
Fig. 2 a, 2b, 2c and 2d are followed successively by ZIF-8 particles 20min, 40min, 60min, 80min growth change in duct
Figure；Fig. 2 e are the schematic diagram of AAO films ion responsitivity experiment；
Fig. 3 is the trend chart of AAO film transmembrane currents；
Fig. 4 reduces trend for AAO membrance currents；
Fig. 5 a, 5b, 5c and 5d are growth change figures of the ZIF-8 in different pore size AAO films；
Fig. 6 a, 6b, 6c and 6d are the comparison diagram of AAO film obverse and reverses before and after reaction.
Reference numeral 1- electrodes, 2- electrolyte, 3- ducts film.
Specific embodiment
As used herein, term "comprising", " comprising ", " containing ", " having " meaning be non-limiting, you can add in
Other steps of result and other ingredients are not influenced.Terms above cover term " by ... form " and " substantially by ... group
Into ".Unless otherwise specified, material, equipment, reagent are commercially available.
The use of solvent is commercially available in the present invention.Zn(NO3)2·6H2O (99% purity), (99% is pure for 2-methylimidazole
Degree), methanol is bought from Aladdin chemical reagent Co., Ltd；AAO films are bought from Whatman and Pu Yuan nanosecond science and technology Co., Ltd
(Hefei, China)；Distilled water is made (resistance value=18.2M Ω cm) by MilliQ systems.
To try to explore the potential application of nano pore, the present invention controls the growth of MOF materials in nanometer confinement space.
Using anodic alumina films (abbreviation AAO films) duct inner wall as substrate grown ZIF-8, the present invention is the method using growth in situ,
ZIF-8 materials are modified in the nano pore in AAO films for the first time.
One aspect of the present invention provides the pattern of anodic alumina films surface nanometer array, the anodised aluminium film surface
The pattern of nano-array is made of the nano-array of pellumina and pellumina surface, and the nano-array is that ZIF-8 receives
Metre hole array, the nano-pore array structure are evenly distributed；The depth in hole is 60 ± 5 μm, and depth-to-width ratio is (4.7 ± 3) × 103。
Another aspect of the present invention provides control such as above-mentioned anodic alumina films surface nanometer array in nanometer confinement space
Pattern growth method, be as follows：
Step 1, stock, Zn (NO3)2·6H2The methanol solution of O, the methanol solution of 2-methylimidazole, the sun of different size
Pole pellumina；Zn(NO3)2·6H2The methanol solution of O is by 5g Zn (NO3)2·6H2O, which is dissolved in 250mL methanol, to be made；2-
The methanol solution of methylimidazole is to be dissolved in 250mL methanol being made by 2.5g 2-methylimidazoles.
Step 2, at room temperature, by Zn (NO3)2·6H2After the methanol solution mixing of the methanol solution and 2-methylimidazole of O
To the reaction solution of ZIF-8；Wherein, Zn (NO3)2·6H2The volume ratio of the methanol solution of O and the methanol solution of 2-methylimidazole is
1:1。
Step 3 after the anodic alumina films of different size are cleaned by ultrasonic 1~5min, is put into Zn (NO3)2·6H2O's
25min~35min is impregnated in methanol solution；The thickness of anodic alumina films is 60 ± 5 μm.Soaking temperature be maintained at 50 DEG C~
60℃。
Step 4 takes out the anodic alumina films of soaking mistake in step 3, blots the solution of film surface, anodic oxidation
Aluminium film is passed through the ZIF-8 reaction solutions prepared in step 2 and is filtered, and ZIF-8 just starts to grow using cell walls as substrate, lasting to take out
Filter, ZIF-8 can be filled in the bulky grain of formation rule in duct gradually.Wherein, it is 50~90min to filter the time.Preferably
The suction filtration time is 55~60min.ZIF-8 grain diameters are 225~252nm in duct.
When ZIF-8 reaction solutions are by duct, since methanol solution is to the wetting capacity of cell walls, ZIF-8 reaction solutions
Cell walls can be attached to, can be quickly formed in cell walls there are many ZIF-8 little particles, in order to which ZIF-8 particles is given to build one
The environment of good continued propagation need to persistently inject fresh ZIF-8 reaction solutions in duct.As fresh ZIF-8 reacts
The lasting injection of liquid, the ZIF-8 little particle continued propagations in cell walls, aggregation gradually form rule, uniform ZIF-8's
Particle is full of in duct.Control, which is injected the time of ZIF-8 reaction solutions and filtered immediately, (prepares fresh ZIF-8 in step 2
Reaction solution, Zn (NO3)2·6H2The methanol solution of O and the methanol solution of 2-methylimidazole keep two kinds of reaction solutions instant
Mixing filters immediately), with regard to the size that can control ZIF-8 and regular degree.Thus it can just be controlled in the nanometer confinement space in duct
The growth of MOF materials processed.
Present invention can apply to anodic alumina films surface nanometer arrays in biophysics, biochemistry, ion detection,
Study the fields such as intermolecular interaction.
The characteristic manner of nano pore
The test of AAO films ion responsitivity experiment is used for using organic glass electrolytic cell, experimental provision to be as shown in Fig. 2 e.
Electrolytic cell is made of two chambers 2, there is functional nano duct film 3 to be fixed among two chambers, chamber cross section
On hole and the contact of film, ion can be detected to pass through duct.Transmembrane current test device be 1 system of bipolar electrode, ion
Using Ag/AgCl electrodes in response test.The operating system of instrument is Keithley Instruments ExceLINX
6487 softwares of software for the Model.With the field sweep voltage of -2V-+2V, detection transmembrane current variation.Test
Electrolyte used is 0.1M KCl solution.
AAO environmental microbes and Cross Section Morphology are characterized by scanning electron microscope NovaNanoSEM200.
The time filtered to AAO films is set to 60min, detects the variation of transmembrane current.Experiment proves to fill in duct
During ZIF-8, transmembrane current can reduce.It can also judge ZIF-8 particles whether are modified in duct by the variation of electric current.It sees
When examining the pattern of ZIF-8 in duct, scanning electron microscope observation AAO films section is utilized.
Examples 1 to 4 is prepared according to the above method, it is as shown in table 1 below,
Table 1 is the reaction condition of Examples 1 to 4
Sectional views of Fig. 1 a for blank AAO films, a diameter of 307 ± 32nm in duct；Fig. 1 b are in situ in AAO fenestras road
Grow the sectional view after ZIF-8, a diameter of 239 ± 13nm of ZIF-8 nano particles.
Fig. 2 a, 2b, 2c, 2d increase for ZIF-8 particles with the suction filtration time and corresponding transmembrane current figure, wherein, Fig. 2 a
For ZIF-8 particles, 20min growth changes figure, Fig. 2 b are ZIF-8 particles 40min growth changes figure in duct in duct, are schemed
2c is ZIF-8 particles 60min growth changes figure in duct, and Fig. 2 d are ZIF-8 particles 80min growth changes figure in duct；
Corresponding transmembrane current variation test device is as shown in Figure 2 e.With the increase for filtering the time, growth in situ in duct
ZIF-8 nanoparticle sizes increase, and lead
The effective aperture in pore road reduces, and electric current reduces.
Fig. 3 is the trend chart for characterizing AAO film transmembrane currents.It in modification after MOF particles, increases over time, MOF
Particle in-situ is grown up, and electric current is caused gradually to decline.
Fig. 4 is changes over time current reduction tendency chart；As seen from Figure 4 when filter the time during 0-40min,
ZIF-8 Grain growths can cause the reduction of the effective aperture in duct, and transmembrane current is made to continue to reduce；When the suction filtration time is in 40-
During 80min, ZIF-8 sizes tend towards stability, and the transmembrane current of AAO films is promoted to tend towards stability.
Experimental result
2 different pore size AAO film ZIF-8 particle size growth situations of table
Fig. 5 a, 5b, 5c and 5d are growth SEM figures of the ZIF-8 in different pore size AAO films；As seen from the figure in difference
In the AAO fenestras road of aperture (as shown in Table 2 above), after ZIF-8 growth in situ in duct same time (60min), particle
Size also differ.
ZIF-8 comparison diagrams of positive (Fig. 6 a and 6b) and reverse side (Fig. 6 c and 6d) before and after being reacted in AAO fenestras road；From
It can be seen from the figure that, ZIF-8 can be grown in AAO ducts, and particle can cover most of hole on AAO to high-density
Road.
To sum up, it can be seen that the time is filtered by control, can effectively control the life of anodic alumina films surface nanometer array
Long speed.And this conclusion can by using organic glass electrolytic cell carry out ion responsitivity experiment to curent change trend into
Row monitoring.
The pattern of anodic alumina films surface nanometer array provided by the present invention and its shape is controlled in nanometer confinement space
The method of looks growth, application, synthetic method is simple, at low cost, and pattern is easy to observation and detection.Obtained nanometer material structure is steady
It is fixed, stable in physicochemical property, and can be recycled.The hole and size of MOF porous materials are very clear and definite, it will assign solid nano
Duct three-dimensional topology property.And nano pore can give MOF materials to provide stable carrier.Anodic oxidation provided by the invention
Aluminium film surface nano-array has larger development potentiality, will be in biophysics, biochemistry, ion detection, and research is intermolecular
Interaction is catalyzed, separation, and the fields such as energy storage are used widely.
The foregoing is merely the preferable specific embodiment of the present invention, but protection scope of the present invention is not limited thereto,
The change or replacement that any one skilled in the art is expected in the technical scope disclosed by the present invention should all be contained
Lid is within protection scope of the present invention.
Claims (10)
1. the pattern of anodic alumina films surface nanometer array, which is characterized in that the anodic alumina films surface nanometer array
Pattern be made of the nano-array of pellumina and pellumina surface, the nano-array is ZIF-8 nanohole arrays,
The nano-pore array structure is evenly distributed；The depth in hole is 60 ± 5 μm, and depth-to-width ratio is (4.7 ± 3) × 103。
2. control what the pattern of anodic alumina films surface nanometer array as described in claim 1 was grown in nanometer confinement space
Method, which is characterized in that be as follows：
Step 1, stock, Zn (NO3)2·6H2The methanol solution of O, the methanol solution of 2-methylimidazole, the anodic oxygen of different size
Change aluminium film；
Step 2, at room temperature, by Zn (NO3)2·6H2It is obtained after the methanol solution mixing of the methanol solution and 2-methylimidazole of O
The reaction solution of ZIF-8；
Step 3 after the anodic alumina films of different size are cleaned by ultrasonic 1~5min, is put into Zn (NO3)2·6H2The methanol of O
25min~35min is impregnated in solution；
Step 4 takes out the anodic alumina films of soaking mistake in step 3, blots the solution of film surface, anodic alumina films
By the ZIF-8 reaction solutions prepared in step 2 and filtering, ZIF-8 just starts to grow using cell walls as substrate, lasting to filter,
ZIF-8 can be filled in the bulky grain of formation rule in duct gradually；Wherein, it is 50~90min to filter the time；
Above-mentioned steps one can control the size and the speed of growth of nano particle to step 4.
3. the pattern growth of anodic alumina films surface nanometer array is controlled in nanometer confinement space as claimed in claim 2
Method, which is characterized in that Zn (NO in the step 13)2·6H2The methanol solution of O is by 5g Zn (NO3)2·6H2O is dissolved in
It is made in 250mL methanol.
4. the pattern growth of anodic alumina films surface nanometer array is controlled in nanometer confinement space as claimed in claim 2
Method, which is characterized in that the methanol solution of 2-methylimidazole is dissolved in by 2.5g 2-methylimidazoles in the step 1
It is made in 250mL methanol.
5. the pattern growth of anodic alumina films surface nanometer array is controlled in nanometer confinement space as claimed in claim 2
Method, which is characterized in that the specification of the anodic alumina films is：71 ± 7.88nm, 100 ± 14.27nm, 249 ±
One or more of 32.97nm and 317 ± 36.17nm；The thickness of anodic alumina films is 60 ± 5 μm.
6. the pattern growth of anodic alumina films surface nanometer array is controlled in nanometer confinement space as claimed in claim 2
Method, which is characterized in that in the step 2, Zn (NO3)2·6H2The methanol solution of O and the methanol solution of 2-methylimidazole
Volume ratio be 1:1.
7. the pattern growth of anodic alumina films surface nanometer array is controlled in nanometer confinement space as claimed in claim 2
Method, which is characterized in that soaking temperature is maintained at 50 DEG C~60 DEG C in the step 3.
8. the pattern growth of anodic alumina films surface nanometer array is controlled in nanometer confinement space as claimed in claim 2
Method, which is characterized in that in the step 4 filter the time be 55~60min.
9. the pattern growth of anodic alumina films surface nanometer array is controlled in nanometer confinement space as claimed in claim 2
Method, which is characterized in that in the step 4 in duct ZIF-8 grain diameters be 225~252nm.
It is 10. a kind of if claim 1~9 any one of them anodic alumina films surface nanometer array is in biophysics, biology
Chemistry, ion detection study intermolecular interaction, are catalyzed, separation, the application in energy storage field.
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| CN109411739A (en) * | 2018-08-31 | 2019-03-01 | 中山大学 | A kind of self power generation, the Zn-CoNC zinc and air cell of long-life and its application |
| CN109411739B (en) * | 2018-08-31 | 2021-06-25 | 中山大学 | Self-generating long-life Zn-CoNC zinc-air battery and application thereof |
| CN109709175A (en) * | 2019-02-25 | 2019-05-03 | 广东海洋大学 | A kind of lead ion detection method based on nanochannel electrochemical sensor |
| CN111118578A (en) * | 2020-01-06 | 2020-05-08 | 南京师范大学 | Electrophoresis-driven two-dimensional metal organic framework nanosheet solid-state nanopore preparation method |
| CN111118578B (en) * | 2020-01-06 | 2021-11-26 | 南京师范大学 | Electrophoresis-driven two-dimensional metal organic framework nanosheet solid-state nanopore preparation method |
| CN111487307A (en) * | 2020-05-07 | 2020-08-04 | 温州大学 | Method for detecting protein based on borosilicate glass nanopores modified by metal organic framework material |
| CN111487307B (en) * | 2020-05-07 | 2023-02-10 | 温州大学 | Method for detecting protein based on borosilicate glass nano-pore channel modified by metal organic framework material |
| CN115181297A (en) * | 2022-06-08 | 2022-10-14 | 中国地质大学（武汉） | AlTCPP @ MOF membrane based on porous alumina nanochannel and preparation method and application thereof |
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