CN102923641B - Method for preparing nano channel with unsymmetrical wettability on two sides - Google Patents
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Abstract
The invention discloses a method for preparing a nano channel with unsymmetrical wettability on two sides. The method comprises the following steps of: preparing a layer of an oxide mesoporous film with photocatalytic performance on one side of a porous anode aluminum oxide nano channel serving as a substrate; modifying super-hydrophobic molecules with super-hydrophobic effects on two sides of the nano channel; and regulating the wettability on one side of the nano channel by ultraviolet irradiation under the photocatalytic action of oxides, so that the wettability on two sides of the nano channel is unsymmetrical. By the unsymmetrical wettability, a rectification effect of the nano channel on ion transmission is realized, and the transmission of ions in the nano channel can be gated.
Description
Technical field
The present invention relates to the preparation method of the asymmetrical nanochannel of a kind of both sides wellability.This nanochannel has ion rectifying effect, and ultraviolet light can the transmission of gate ion.Belong to technical field of function materials.
Background technology
Ion channel on cell membrane carries out a series of vital movement to organism and plays vital effect, and its special 26S Proteasome Structure and Function causes the extensive concern of Chinese scholars.The artificial nano passage of different-shape and function prepared by people's mimic biology body ion channel, and these nanochannels are in design and prepare novel sensor, the field such as detection of flow device and DNA received all shows certain application space, see bibliography [1-3].Bibliography [1]: R.Wei, V.Gatterdam, R.Wieneke, R.Tamp é and U.Rant, Stochastic sensing of proteins with receptor-modified solid-statenanopores.Nat.Nanotechnol., 2012,7,257 – 263. bibliography [2]: Q.Zhang, Z.Liu, X.Hou, X.Fan, J.Zhai and L.Jiang, Light-regulated ion transport through artificial ion channels based on TiO
2nanotubular arrays.Chem.Commun., 2012,48,5901 – 5903. bibliography [3]: S.Iqbal, D.Akin, R.Bashir, Solid-state nanopore channels with DNA selectivity.Nat.Nanotechnol., 2007,2,243 – 248.
Compared with biological duct, artificial nano channel material not only has the unappeasable stable physical property of biomaterial, and has the controllability of shape and surface chemistry composition, so just provides good research platform for design and development intelligent nano passage.In general, the main thought of constructing bionic nano passage is exactly the asymmetry realizing passage.At present, the asymmetry of common artificial bionic nanochannel mainly comprises that structure is asymmetric, surface chemistry composition is asymmetric, internal charge distribution is asymmetric.
Summary of the invention
Main purpose of the present invention is to propose the new asymmetric method of modifying of a kind of nanochannel, prepare the asymmetrical nanochannel of a kind of both sides wellability, achieve the ion rectifying effect of nanochannel, and the transmission of gate ion can be carried out by Illumination adjusting.
The present invention adopts the method for evaporation induced self-assembly, is uniformly mixed by the reactants such as presoma, template, organic solvent and ageing formation gel, is coated with by gel in porous anodic aluminium oxide (AAO) substrate; After dry process, within 1 ~ 4 hour, obtaining at 300 ~ 500 ° of C temperature lower calcinations with AAO is the oxide mesoporous film of substrate; Finally, the molecule with super hydrophobic functional is all modified in the inside of nanotube films and surface; Make the super hydrophobic functional molecular breakdown of oxide mesoporous film side change wellability by UV-irradiation, and AAO side remain super-hydrophobic state, can obtain the asymmetrical nanochannel of both sides wellability.
The invention provides the preparation method of the asymmetrical nanochannel of a kind of both sides wellability, by weight percentage, the concrete steps of the method comprise:
The first step, take porous anodic aluminium oxide as substrate, prepares oxide mesoporous film in substrate side:
If described oxide mesoporous film is titanium dioxide mesoporous film, then preparation process is:
(1) at room temperature, the template of 1 ~ 5% is dissolved in 50 ~ 70% organic solvents, forms the first mixed liquor; A kind of titanium source of 10 ~ 30% and the concentrated hydrochloric acid (36wt%) of 10 ~ 20% are uniformly mixed, or the titanium source of the titanium tetrachloride of 10 ~ 20% and 20 ~ 40% is uniformly mixed, form the second mixed liquor.In above-mentioned first mixed liquor and the second mixed liquor, the percentage by weight sum of each component is 100%.
(2) by above-mentioned two kind of first mixed liquor and the second mixed liquor mix and blend 2 ~ 5 hours; Be 10 ~ 30 ° of C in temperature, leave standstill 1 ~ 3 day under the condition of humidity 30 ~ 100%, obtain gel.
(3) above-mentioned gel is coated with in porous anodic aluminium oxide (AAO) substrate; Within 1 ~ 4 hour, obtain with AAO being the titanium dioxide mesoporous film of substrate in 300 ~ 500 ° of C temperature lower calcinations after dry process under 40 ~ 100 ° of C.
If described oxide mesoporous film is zinc oxide mesopore film, then preparation process is:
A under () room temperature, be dissolved in the ethanol of 50 ~ 60% by the zinc acetate of 4 ~ 5%, the template adding 2 ~ 3% under vigorous stirring makes it to dissolve, and forms the first mixed liquor; The lithium hydroxide of 2 ~ 4% is dissolved in the ethanol of 30 ~ 40%, forms the second mixed liquor.In above-mentioned first mixed liquor and the second mixed liquor, the percentage by weight sum of each component is 100%.
(b) by above-mentioned two kind of first mixed liquor and the second mixed liquor mix and blend 2 ~ 3 hours, whipping temp 60 ° of C; Then be 20 ~ 30 ° of C in temperature, leave standstill 1 ~ 2 day under the condition of humidity 30 ~ 40%, obtain gel;
C above-mentioned gel is coated with in porous anodic aluminium oxide substrate by (); Within 1 ~ 3 hour, zinc oxide mesopore film is obtained in 300 ~ 400 ° of C temperature lower calcinations after dry process under 60 ~ 100 ° of C.
Second step, 30 ~ 50 μ g super hydrophobic functional molecules are instilled in pyroreaction still, above-mentioned oxide mesoporous film is put into pyroreaction still, reacts 2 ~ 4 hours at 100 ~ 150 ° of C temperature, can by super hydrophobic functional molecular modification on oxide mesoporous film.
3rd step, change its wellability by the time changing the oxide mesoporous film side of UV-irradiation, opposite side wellability remains unchanged, and namely obtains the asymmetrical nanochannel of both sides wellability.
Described organic solvent is the organic solvents such as oxolane, ethanol or n-butanol, is AR.
Described titanium source is the organic titanate such as titanate esters (butyl titanate, tetraethyl titanate or isopropyl titanate) or titanium ethanolate.
Described template is polyoxyethylene-poly-oxypropylene polyoxyethylene (PEO-PPO-PEO) triblock copolymer that the degree of polymerization is different: P123(weight average molecular weight M
wbe about 5800), F108(weight average molecular weight M
wbe about 14600) or F127(weight average molecular weight M
wbe about 12600).
Described super hydrophobic functional molecule is octadecylsilane (ODS), octadecyl trimethoxysilane (OTS) or silicon fluoride (FAS-3, FAS-13, FAS-17) etc.
The invention has the advantages that:
1, the invention provides a kind of nanochannel Novel asymmetric method of modifying;
2, the porous nano passage that the present invention prepares has the typical rectifying effect being similar to Prof. Du Yucang single hole nanochannel, and the electric current that passage is larger and rectifying effect make it have practical application space widely;
3, the commutating ratio by regulating the UV-irradiation time can change nanochannel.
Accompanying drawing explanation
Fig. 1. AAO substrate surface ESEM (SEM) pattern top view of the present invention and sectional drawing (illustration);
Fig. 2. nanochannel surface SEM pattern top view of the present invention and sectional drawing (illustration);
Fig. 3. nanochannel surface transmission Electronic Speculum (TEM) shape appearance figure of the present invention;
Fig. 4. nanochannel both sides contact angle of the present invention and the relation curve of UV-irradiation time;
Fig. 5. the current-voltage curve of nanochannel of the present invention after the different UV-irradiation time;
Fig. 6. the present invention modifies nanochannel commutating ratio before and after super hydrophobic functional molecule and the relation curve of UV-irradiation time;
Fig. 7. gas current testing arrangement figure of the present invention.
Detailed description of the invention
Below in conjunction with drawings and Examples, technical scheme of the present invention is further described:
embodiment 1:
The first step, at room temperature, is dissolved in the P123 of 1% in 50% tetrahydrofuran solvent, forms the first mixed liquor; The concentrated hydrochloric acid (36wt%) of the butyl titanate of 29% and 20% is uniformly mixed, forms the second mixed liquor.
Second step, by above-mentioned two kinds of mixed liquor mix and blends 2 hours; Be 25 ° of C in temperature, leave standstill 1 day under the condition of humidity 30%, obtain gel.
3rd step, is coated with above-mentioned gel in porous anodic aluminium oxide (AAO) substrate; Under 60 ° of C, after dry process, under 300 ° of C, calcining obtains with AAO being the titanium dioxide mesoporous film of substrate for 4 hours.
4th step, instills 30 μ g octadecyl trimethoxysilane (OTS), puts into wherein by above-mentioned titanium dioxide mesoporous film in pyroreaction still, reacts 4 hours, OTS can be modified on titanium dioxide mesoporous film under 100 ° of C.
5th step, change its wellability by the time changing UV-irradiation titanium dioxide side, opposite side wellability remains unchanged, and namely obtains the asymmetrical nanochannel of both sides wellability.Irradiation time is not more than 120min.
embodiment 2:
(1) at room temperature, the F127 of 3% is dissolved in 52% ethanol; The concentrated hydrochloric acid (36wt%) of the isopropyl titanate of 30% and 15% is uniformly mixed.
(2) by above-mentioned two kinds of mixed liquor mix and blends 3 hours; Be 10 ° of C in temperature, leave standstill 2 days under the condition of humidity 80%, obtain gel.
(3) above-mentioned gel is coated with in porous anodic aluminium oxide (AAO) substrate; Under 80 ° of C, after dry process, under 400 ° of C, calcining obtains with AAO being the titanium dioxide mesoporous film of substrate for 3 hours.
(4) in pyroreaction still, instill 40 μ g octadecylsilane (ODS), above-mentioned titanium dioxide mesoporous film is put into wherein, react 2 hours under 150 ° of C, ODS can be modified on titanium dioxide mesoporous film.
(5) time by changing UV-irradiation titanium dioxide side changes its wellability, and opposite side wellability remains unchanged, and namely obtains the asymmetrical nanochannel of both sides wellability.Irradiation time is not more than 120min.
embodiment 3:
(1) at room temperature, the F108 of 5% is dissolved in the n-butanol of 70%; The concentrated hydrochloric acid (36wt%) of the titanium ethanolate of 15% and 10% is uniformly mixed.
(2) by above-mentioned two kinds of mixed liquor mix and blends 4 hours; Be 20 ° of C in temperature, leave standstill 3 days under the condition of humidity 60%, obtain gel.
(3) above-mentioned gel is coated with in porous anodic aluminium oxide (AAO) substrate; Under 40 ° of C, after dry process, under 450 ° of C, calcining obtains with AAO being the titanium dioxide mesoporous film of substrate for 2 hours.
(4) in pyroreaction still, instill 50 μ g silicon fluorides (FAS-13), above-mentioned titanium dioxide mesoporous film is put into wherein, react 3 hours under 130 ° of C, FAS-13 can be modified on titanium dioxide mesoporous film.
(5) time by changing UV-irradiation titanium dioxide side changes its wellability, and opposite side wellability remains unchanged, and namely obtains the asymmetrical nanochannel of both sides wellability.Irradiation time is not more than 120min.
embodiment 4:
(1) at room temperature, the F108 of 2% is dissolved in the ethanol of 68%; The titanium tetrachloride of 10% and the isopropyl titanate of 20% are uniformly mixed.
(2) by above-mentioned two kinds of mixed liquor mix and blends 5 hours; Be 30 ° of C in temperature, leave standstill 3 days under the condition of humidity 100%, obtain gel.
(3) above-mentioned gel is coated with in porous anodic aluminium oxide (AAO) substrate; Under 80 ° of C, after dry process, under 500 ° of C, calcining obtains with AAO being the titanium dioxide mesoporous film of substrate for 1 hour.
(4) in pyroreaction still, instill 45 μ g silicon fluorides (FAS-17), above-mentioned perforated membrane is put into wherein, react 3.5 hours under 120 ° of C, FAS-17 can be modified on perforated membrane.
(5) time by changing UV-irradiation titanium dioxide side changes its wellability, and opposite side wellability remains unchanged, and namely obtains the asymmetrical nanochannel of both sides wellability.Irradiation time is not more than 120min.
embodiment 5:
(1) under room temperature, be dissolved in the ethanol of 60% by the zinc acetate of 5%, the F127 adding 3% under vigorous stirring makes it to dissolve; The lithium hydroxide of 2% is dissolved in the ethanol of 30%.
(2) by above-mentioned two kinds of mixed liquors mixing, under 60 ° of C, stirring reaction filtered after 3 hours; Be 30 ° of C in temperature, leave standstill 1 day under the condition of humidity 40%, obtain gel.
(3) above-mentioned gel is coated with in porous anodic aluminium oxide (AAO) substrate; Under 100 ° of C, after dry process, under 400 ° of C, calcining obtains with AAO being the zinc oxide mesopore film of substrate for 2 hours.
(4) in pyroreaction still, instill 30 μ g octadecyl trimethoxysilane (OTS), above-mentioned zinc oxide mesopore film is put into wherein, react 2 hours under 150 ° of C, OTS can be modified on zinc oxide mesopore film.
(5) time by changing UV-irradiation zinc oxide side changes its wellability, and opposite side wellability remains unchanged, and namely obtains the asymmetrical nanochannel of both sides wellability.Irradiation time is not more than 120min.
embodiment 6:
(1) under room temperature, be dissolved in the ethanol of 50% by the zinc acetate of 4%, the P123 adding 2% under vigorous stirring makes it to dissolve; The lithium hydroxide of 4% is dissolved in the ethanol of 40%.
(2) by above-mentioned two kinds of mixed liquors mixing, under 60 ° of C, stirring reaction filtered after 3 hours; Be 20 ° of C in temperature, leave standstill 2 days under the condition of humidity 30%, obtain gel.
(3) above-mentioned gel is coated with in porous anodic aluminium oxide (AAO) substrate; Under 60 ° of C, after dry process, under 300 ° of C, calcining obtains with AAO being the zinc oxide mesopore film of substrate for 1 hour.
(4) in pyroreaction still, instill 35 μ g silicon fluorides (FAS-17), above-mentioned zinc oxide mesopore film is put into wherein, react 4 hours under 100 ° of C, OTS can be modified on zinc oxide mesopore film.
(5) time by changing UV-irradiation zinc oxide side changes its wellability, and opposite side wellability remains unchanged, and namely obtains the asymmetrical nanochannel of both sides wellability.Irradiation time is not more than 120min.
Select the nanochannel obtained in above-described embodiment to carry out morphology observation, and the nanochannel both sides contact angle after different time UV-irradiation and gas current tested:
1, the pattern of nanochannel:
The surface of AAO substrate and sectional drawing as shown in Figure 1, AAO perforated membrane have densely distributed, arrange regular straight hole, average pore size is about 100nm.As can be seen from Figure 2: the hole of AAO substrate surface is covered by one deck sull completely, sull is relatively more even and defect is less, and the thickness of sull is about 1.3 μm, and the thickness of AAO perforated membrane is about 56 μm.Because the aperture of sull is extremely small, be difficult to observe by SEM, so its surface topography will be observed by transmission electron microscope, as can be seen from Figure 3: sull is the mesopore film that one deck aperture is about 6nm.The nanochannel that the present invention prepares is porous membrane passage, and these passages are that the circulation of gas current test process effects of ion provides path.
2, the test of contact angle:
Be the both sides of the UV-irradiation nanochannel of 365nm with wavelength, irradiation time extends to 120min gradually; After each irradiation, measure the contact angle values of nanochannel both sides with contact angle measurement, contact angle with light application time change as shown in Figure 4.Nanochannel AAO side contact angle without UV-irradiation is about 150 °, TiO
2side is about 140 °, and owing to having modified super hydrophobic functional molecule, both sides all show stronger hydrophobicity.After UV-irradiation, TiO
2side contact angle significantly declines, and the decreasing value of irradiating the contact angle after 30min is about 70 °, and along with the UV-irradiation time continues to extend, contact angle change is slow gradually, and during illumination 120min, contact angle almost remains unchanged; After UV-irradiation, AAO side contact angle is about 140 °, and along with UV-irradiation time lengthening, contact angle is almost unchanged, and namely AAO side remains good hydrophobicity.This is due to TiO
2there is excellent photocatalysis performance, after UV-irradiation, TiO
2the OTS of side decomposes in a large number, its surface from hydrophobic become hydrophilic; And AAO does not possess this performance, its surperficial OTS can not decompose under UV-irradiation, and wellability is constant, and therefore contact angle almost remains unchanged.
3, the test of gas current:
Nanochannel is fixed in the middle of gas current test pool, both sides add potassium chloride electrolyte solution respectively, and use two Ag/AgCl electrodes to apply membrane potential, positive pole is positioned at nanochannel AAO side, with the gas current of picoammeter test by nanochannel, testing arrangement as shown in Figure 7.In test process, irradiate nanochannel ZnO or TiO respectively with the ultraviolet light of different time
2side, apply the scanning potential test of-0.2V to+0.2V after each irradiation in nanochannel both sides by the gas current of nanochannel, obtain current-voltage curve, test result is shown in Fig. 5.
(a) current-voltage curve:
In Fig. 5, curve a is the I-V characteristic curve of the nanochannel without UV-irradiation, and curve b to curve f is respectively after UV-irradiation also extends irradiation time gradually, the I-V characteristic curve of nanochannel.As seen from the figure, nanochannel gas current without UV-irradiation is very little, this is that nanochannel both sides owing to modifying super-hydrophobic molecule all show stronger hydrophobicity, passage is almost in non-conducting state, ion is difficult to by nanochannel, so gas current is almost 0(curve a).Extend irradiation time through UV-irradiation, increased gradually by the gas current of nanochannel and occur certain rectification characteristic (curve b-curve f).This is that super-hydrophobic molecule is due to TiO due under UV-irradiation
2photocatalysis and decompose, nanochannel one side surface becomes hydrophily from stronger hydrophobic state, hydrophobic layer thickness reduce, resistance reduce gas current increase.
B () commutating ratio calculates:
The ratio calculation of the current absolute value corresponding by negative sense maximum voltage and forward maximum voltage corresponding current value can obtain the gas current commutating ratio by nanochannel after different time UV-irradiation, and corresponding result of calculation as shown in Figure 6.Can be found out by the relation curve of commutating ratio and irradiation time: nanochannel commutating ratio after the UV-irradiation of different time of the super-hydrophobic molecule of unmodified is all about 1, namely without rectifying effect.Modify the nanochannel after super-hydrophobic molecule and be about 1 without commutating ratio during UV-irradiation, occur without rectifying effect; And after ultraviolet light short irradiation, there is obvious rectifying effect, commutating ratio reaches about 2.8.Along with the increase of UV-irradiation time, commutating ratio is decreased to about 1.2 gradually, and rectifying effect becomes not obvious.
By drawing the test of nanochannel contact angle, gas current under different time UV-irradiation and the calculating of commutating ratio: the present invention achieves the gate control function of passage by changing the infiltrating difference in nanochannel both sides, and the typical rectification characteristic of nanochannel after obtaining the asymmetric modification of wellability; By the change of light application time, the commutating ratio size of nanochannel can be made to change.
Claims (5)
1. a preparation method for the asymmetrical nanochannel of both sides wellability, is characterized in that: comprise following step:
The first step, take porous anodic aluminium oxide as substrate, prepares oxide mesoporous film in substrate side;
By weight percentage, when described oxide mesoporous film is titanium dioxide mesoporous film, the step of concrete preparation is:
A the template of 1 ~ 5% at room temperature, is dissolved in 50 ~ 70% organic solvents by (), form the first mixed liquor; The titanium source of 10 ~ 30% and the concentrated hydrochloric acid of 10 ~ 20% are uniformly mixed, or the titanium source of the titanium tetrachloride of 10 ~ 20% and 20 ~ 40% is uniformly mixed, form the second mixed liquor; In above-mentioned first mixed liquor and the second mixed liquor, the percentage by weight sum of each component is 100%;
B () is by above-mentioned two kind of first mixed liquor and the second mixed liquor mix and blend 2 ~ 5 hours; Be 10 ~ 30 DEG C in temperature, leave standstill 1 ~ 3 day under the condition of humidity 30 ~ 100%, obtain gel;
C above-mentioned gel is coated with in porous anodic aluminium oxide substrate by (); Within 1 ~ 4 hour, oxide mesoporous film is obtained in 300 ~ 500 DEG C of temperature lower calcinations after dry process at 40 ~ 100 DEG C;
By weight percentage, when described oxide mesoporous film is zinc oxide mesopore film, the step of concrete preparation is:
A under () room temperature, be dissolved in the ethanol of 50 ~ 60% by the zinc acetate of 4 ~ 5%, the template adding 2 ~ 3% under vigorous stirring makes it to dissolve, and forms the first mixed liquor; The lithium hydroxide of 2 ~ 4% is dissolved in the ethanol of 30 ~ 40%, forms the second mixed liquor; In above-mentioned first mixed liquor and the second mixed liquor, the percentage by weight sum of each component is 100%;
(b) by above-mentioned two kind of first mixed liquor and the second mixed liquor mix and blend 2 ~ 3 hours, whipping temp 60 DEG C; Then be 20 ~ 30 DEG C in temperature, leave standstill 1 ~ 2 day under the condition of humidity 30 ~ 40%, obtain gel;
C above-mentioned gel is coated with in porous anodic aluminium oxide substrate by (); Within 1 ~ 3 hour, zinc oxide mesopore film is obtained in 300 ~ 400 DEG C of temperature lower calcinations after dry process at 60 ~ 100 DEG C;
Described organic solvent is oxolane, ethanol or n-butanol; Described template is the polyoxyethylene-poly-oxypropylene polyoxyethylene triblock copolymer that the degree of polymerization is different;
Second step, instills 30 ~ 50 μ g super hydrophobic functional molecules, above-mentioned oxide mesoporous film is put into pyroreaction still in pyroreaction still, reacts 2 ~ 4 hours, at 100 ~ 150 DEG C of temperature by super hydrophobic functional molecular modification on oxide mesoporous film;
3rd step, change its wellability by the time changing the oxide mesoporous film side of UV-irradiation, opposite side wellability remains unchanged, and namely obtains the asymmetrical nanochannel of both sides wellability, and oxide mesoporous membrane pore size is 6nm.
2. the preparation method of the asymmetrical nanochannel of a kind of both sides wellability according to claim 1, is characterized in that: the concentration of described concentrated hydrochloric acid is 36wt%.
3. the preparation method of the asymmetrical nanochannel of a kind of both sides wellability according to claim 1, is characterized in that: described titanium source is butyl titanate, tetraethyl titanate, isopropyl titanate or titanium ethanolate.
4. the preparation method of the asymmetrical nanochannel of a kind of both sides wellability according to claim 1, is characterized in that: described triblock copolymer is P123, weight average molecular weight M
wbe 5800; Or be F108, weight average molecular weight M
wbe 14600; Or be F127, weight average molecular weight M
wbe 12600.
5. the preparation method of the asymmetrical nanochannel of a kind of both sides wellability according to claim 1, is characterized in that: described super hydrophobic functional molecule is octadecylsilane, octadecyl trimethoxysilane or silicon fluoride.
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| CN116082064A (en) * | 2021-11-08 | 2023-05-09 | 复旦大学 | Mesoporous titanium dioxide/anodic aluminum oxide heterogeneous nano channel and preparation method thereof |
| CN114314654B (en) * | 2021-12-29 | 2022-10-18 | 复旦大学 | Super-assembly preparation method of 4-aminothiophenol modified titanium dioxide heterojunction film |
| CN114950589B (en) * | 2022-05-27 | 2024-02-09 | 复旦大学 | Application of MCT/AAO heterogeneous ultrathin film in light-operated bidirectional adjustable ion transmission |
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