CN105887158A - Nanocrystalline metal oxide array with under-oil super-hydrophobicity and super-hydrophilicity reversible transition function and preparation method thereof - Google Patents
Nanocrystalline metal oxide array with under-oil super-hydrophobicity and super-hydrophilicity reversible transition function and preparation method thereof Download PDFInfo
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- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
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Abstract
The invention discloses a nanocrystalline metal oxide array with an under-oil super-hydrophobicity and super-hydrophilicity reversible transition function and a preparation method thereof. The static contact angle under the oil phase is larger than 150 degrees after the nanocrystalline metal oxide array is subjected to thermal treatment at the temperature ranging from 120 DEG C to 350 DEG C for 1 h to 4 h, and the nanocrystalline metal oxide array has super-hydrophobicity performance; the static contact angle of water under the oil phase is smaller than 10 degrees after the nanocrystalline metal oxide array is irradiated under ultraviolet light for 1 h to 2 h, the nanocrystalline metal oxide array has super-hydrophilicity performance, and the conversion from super-hydrophobicity to super-hydrophilicity is achieved; and after heating recovery is conducted for 1.5 h to 3 h at the temperature ranging from 100 DEG C to 150 DEG C, the static contact angle of water under the oil phase recovers to 150 degrees or above, the nanocrystalline metal oxide array has super-hydrophobicity performance, and the reversible conversion from super-hydrophilicity to super-hydrophobicity is achieved. According to the method, the nanocrystalline metal oxide array is prepared through an existing mature and simple method and is subjected to the processes of thermal treatment, ultraviolet irradiation and heating recovery, the function of reversible conversion from super-hydrophobicity to super-hydrophilicity under different oil phase complex environments is achieved, and therefore the application range of nanotube array intelligent conversion is widened, and important application prospects are achieved.
Description
Technical field
The present invention relates to a kind of nano-metal-oxide array under oil phase environment with super-hydrophobic and super hydrophilic reversible transition function and preparation method thereof.
Background technology
In recent years, by this environmental stimuli, there is the nano-array of this reversible moistened surface sex reversal and caused the extensive concern of people, owing to it has potential application in every field.Conductor oxidate, due to the energy gap that it is higher, can be widely used in photoelectron, photocatalysis and wellability field, and be studied widely by scholars.1997 years, reported first TiO2Nanoparticle is aerial to be had by the hydrophobic function to super hydrophilic reversible transition, also has scholar to use ZnO nano-rod array successfully to achieve the most super-hydrophobic function to super hydrophilic reversible transition.But for the semiconductor nano metal-oxide array that presently, there are by the super-hydrophobic the rarest research of realization to super hydrophilic this function of reversible transition.
Summary of the invention
In order to solve the problems referred to above, the invention provides and a kind of there is nano-metal-oxide array of super-hydrophobic and super hydrophilic reversible transition function and preparation method thereof under oil.Nano-metal-oxide array, after Overheating Treatment, has ultra-hydrophobicity under oil, and the static contact angle of water is more than 150 °, and after ultraviolet light irradiates, the static contact angle at You Xiashui is less than 10 °, has super hydrophilicity;Replying through heating, this nano-metal-oxide array is returned to again more than 150 ° at the static contact angle of You Xiashui, has again ultra-hydrophobicity again, it is achieved thereby that by the super-hydrophobic function to super hydrophilic reversible transition under oil.Simultaneously, prepared by the present invention has the nano-metal-oxide array of super-hydrophobic and super hydrophilic reversible transition function under oil, in the complex environments such as different oil phases, all can realize this under oil by the super-hydrophobic function to super hydrophilic reversible transition, repeatedly reversible transition can be carried out simultaneously.
It is an object of the invention to be achieved through the following technical solutions:
A kind of have the nano-metal-oxide array of super-hydrophobic and super hydrophilic reversible transition function under oil, and described nano-metal-oxide array is TiO2Nano-tube array, WO3Nano-tube array or ZnO nano-rod array, after it carries out heat treatment 1 ~ 4h at 120 ~ 350 DEG C, under oil phase, static contact angle is more than 150 °, has ultra-hydrophobicity;Under ultraviolet light irradiates after 1 ~ 2h, under oil phase, the static contact angle of water is less than 10 °, has super hydrophilicity, it is achieved by the super-hydrophobic function to super hydrophilic transformation;After heating reply 1.5 ~ 3h under the conditions of temperature is 100 ~ 150 DEG C, under oil phase, the static contact angle of water is returned to more than 150 °, has ultra-hydrophobicity, it is achieved by the super hydrophilic function to super-hydrophobic reversible transition.
A kind of have the preparation method of the nano-metal-oxide array of super-hydrophobic and super hydrophilic reversible transition function under oil, comprises the steps:
One, the preparation of nano-metal-oxide array:
Anodizing is used to prepare TiO2And WO3Nano-tube array, uses electrochemical deposition method to prepare ZnO nano-rod array.
With TiO2As a example by nano-tube array, its preparation method is as follows: using ethylene glycol, ammonium fluoride and the mixed electrolytic solution of deionized water, with metal as anode, platinized platinum is negative electrode, prepares TiO by the method for two-step anodization2Nano-tube array.
In this step, in described mixed electrolytic solution, the volume ratio of ethylene glycol, ammonium fluoride and deionized water is 98:0.3:2;Described metal be titanium sheet (Ti) described oxidation voltage be 30 ~ 50V, oxidization time is 1 ~ 3h.
Two, the nano-metal-oxide array of preparation is carried out heat treatment 1 ~ 4h at 120 ~ 350 DEG C, it is achieved that the static contact angle of water is more than 150 ° under oil phase, has ultra-hydrophobicity.
In this step, in addition to normal hexane, thermally treated nano-metal-oxide array static contact angle of water under the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane is all higher than 150 °, it is achieved that also have ultra-hydrophobicity under different oil phase complex environments.
In this step, in above-mentioned oil phase, the water using pH to be 0 ~ 14 measures its static contact angle and is more than 150 °, and nano-metal-oxide array also has ultra-hydrophobicity, embodies its acid-proof alkaline.
Three, by the nano-metal-oxide array after step 2 heat treatment, clean through deionized water rinsing, dry up, 1 ~ 2h under ultraviolet light irradiates, under oil phase, the static contact angle of water is less than 10 °, has super hydrophilicity, it is achieved that by the super-hydrophobic function to super hydrophilic transformation.
In this step, oil phase is in addition to normal hexane, nano-metal-oxide array its static contact angle of water in the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane irradiated through ultraviolet light is less than 10 °, it is achieved by the super-hydrophobic function to super hydrophilic transformation under different oil phase complex environments.
In this step, under above-mentioned oil phase, the water using pH to be 0 ~ 14 measures its static contact angle again smaller than 10 °, and nano-metal-oxide array the most also has ultra-hydrophobicity, embodies it by super-hydrophobic acid-proof alkaline in super hydrophilic transition process.
Four, the nano-metal-oxide array after step 3 ultraviolet light being irradiated, same clean through deionized water rinsing, dry up, it it is 100 ~ 150 DEG C in temperature, heating reply 1.5 ~ 3h, the static contact angle of water under oil phase can be realized and be returned to again more than 150 °, there is again ultra-hydrophobicity, it is achieved that by the super hydrophilic function to super-hydrophobic reversible transition.
In this step, oil phase is in addition to normal hexane, heated rear nano-metal-oxide array its static contact angle of water in the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane is less than 10 °, it is achieved that by the super hydrophilic function to super-hydrophobic reversible transition under different oil phase complex environments.
In this step, in above-mentioned oil phase, the water using pH to be 0 ~ 14 measures its static contact angle again smaller than 10 °, and nano-metal-oxide array the most also has ultra-hydrophobicity, embodies it by super hydrophilic acid-proof alkaline during super-hydrophobic reversible transition.
Five, repeat step three and four, carry out the most super-hydrophobic and super hydrophilic reversible transition.
In this step, the number of times of described the most super-hydrophobic and super hydrophilic reversible transition is at least 4 times.
Present invention have the advantage that
The present invention uses existing ripe straightforward procedure to prepare nano-metal-oxide array, thermally treated, ultraviolet light irradiates and heating Recovery Process, achieve under different oil phase complex environments by the super-hydrophobic function to super hydrophilic reversible transition, therefore the present invention has widened nano-tube array intelligence Transformation Application scope, has important application prospect.
Accompanying drawing explanation
Fig. 1 is TiO prepared by anodic oxidation2Nano-tube array SEM schemes;
Fig. 2 is initial TiO after heat treatment2The static contact angle picture of water under nano-array oil phase;
Fig. 3 is TiO after ultraviolet light irradiates2The static contact angle picture of water under nano-tube array oil phase;
Fig. 4 is TiO after heating reply2The static contact angle picture of water under nano-tube array oil;
Fig. 5 is TiO2Nano-tube array is changed block diagram by super-hydrophobic to the static contact angle of super hydrophilic reversible transition water under different oil phase complex environments;
Fig. 6 is TiO2Nano-tube array is changed block diagram by super-hydrophobic to the static contact angle of super hydrophilic reversible transition difference pH water under oil.
Detailed description of the invention
Below in conjunction with the accompanying drawings technical scheme is further described; but it is not limited thereto; every technical solution of the present invention is modified or equivalent, without deviating from the spirit and scope of technical solution of the present invention, all should contain in protection scope of the present invention.
Embodiment
1
A kind of nano-metal-oxide array specific embodiments with super-hydrophobic and super hydrophilic reversible transition function under oil is as follows:
One, the preparation of nano-metal-oxide array: the ratio using ethylene glycol, ammonium fluoride and deionized water is 98vol%:0.3wt%:2vol% mixed electrolytic solution, with metal Ti sheet as anode, platinized platinum is negative electrode, and anodic oxidation voltage is 30V, oxidization time is 3h, obtains TiO2Nano-tube array, as shown in Figure 1.
Two, by the TiO of preparation2Nano-tube array carries out heat treatment 4h at 120 DEG C, it is achieved that under normal hexane oil phase, the static contact angle of water is more than 150 °, has ultra-hydrophobicity, as shown in Figure 2.
In this step, in addition to normal hexane, thermally treated TiO2Nano-tube array static contact angle of water under the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane is all higher than 150 °, it is achieved also have ultra-hydrophobicity, as shown in Figure 5 under different oil phase complex environments.
In this step, in the above-mentioned oil phase of institute, the water using pH to be 0 ~ 14 measures its static contact angle and is more than 150 °, TiO2Nano-tube array also has super-hydrophobicity, embodies its acid-proof alkaline real, as shown in Figure 6.
Three, by the TiO after above-mentioned steps two heat treatment2Nano-tube array, clean through deionized water rinsing, dry up, 1h under ultraviolet light irradiates, under normal hexane oil phase, the static contact angle of water is less than 10 °, has super hydrophilicity, it is achieved that by the super-hydrophobic function to super hydrophilic transformation, as shown in Figure 3.
In this step, in addition to normal hexane, through the TiO that ultraviolet light irradiates2Nano-tube array its static contact angle of water in the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane is less than 10 °, it is achieved that by the super-hydrophobic function to super hydrophilic transformation under different oil phase complex environments, as shown in Figure 5.
In this step, under above-mentioned oil phase, the water using pH to be 0 ~ 14 measures its static contact angle again smaller than 10 °, TiO2Nano-tube array the most also has ultra-hydrophobicity, embody its by super-hydrophobic acid-proof alkaline in super hydrophilic transition process, as shown in Figure 6.
Four, the TiO after above-mentioned steps three ultraviolet light being irradiated2Nano-tube array, clean through deionized water rinsing equally, dry up, it is 100 DEG C in temperature, heats 3h, the static contact angle of water under normal hexane oil phase can be realized and be returned to again more than 150 °, there is again ultra-hydrophobicity, it is achieved that by the super hydrophilic function to super-hydrophobic reversible transition, as shown in Figure 4.
In this step, in addition to normal hexane, heated rear TiO2Nano-tube array its static contact angle of water in the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane is more than 150 °, it is achieved that by the super hydrophilic function to super-hydrophobic reversible transition in complex environment, as shown in Figure 5.
In this step, in above-mentioned oil phase, the water using pH to be 0 ~ 14 measures its static contact angle and is more than 150 °, embodies TiO2Nano-tube array is by super hydrophilic acid-proof alkaline during super-hydrophobic reversible transition, as shown in Figure 6.
In the present embodiment, TiO2Nano-tube array can realize at least 4 reversible transitions.
Embodiment
2
A kind of nano-metal-oxide array specific embodiments with super-hydrophobic and super hydrophilic reversible transition function under oil is as follows:
One, the preparation of nano-metal-oxide array: the ratio using ethylene glycol, ammonium fluoride and deionized water is 98vol%:0.3wt%:2vol% mixed electrolytic solution, with metal Ti sheet as anode, platinized platinum is negative electrode, use two-step anodization, each oxidation voltage is 50V, oxidization time is 1h, obtains TiO2Nano-tube array, as shown in Figure 1.
Two, by the TiO of preparation2Nano-tube array carries out heat treatment 1h at 350 DEG C, it is achieved that under normal hexane oil phase, the static contact angle of water is more than 150 °, has ultra-hydrophobicity, as shown in Figure 2.
In this step, in addition to normal hexane, thermally treated TiO2Nano-tube array static contact angle of water under the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane is all higher than 150 °, it is achieved also have ultra-hydrophobicity, as shown in Figure 5 under different oil phase complex environments.
In this step, in the above-mentioned oil phase of institute, the water using pH to be 0 ~ 14 measures its static contact angle and is more than 150 °, TiO2Nano-tube array also has super-hydrophobicity, embodies its acid-proof alkaline real, as shown in Figure 6.
Three, by the TiO after above-mentioned steps two heat treatment2Nano-tube array, clean through deionized water rinsing, dry up, 2h under ultraviolet light irradiates, under normal hexane oil phase, the static contact angle of water is less than 10 °, has super hydrophilicity, it is achieved that by the super-hydrophobic function to super hydrophilic transformation, as shown in Figure 3.
In this step, in addition to normal hexane, through the TiO that ultraviolet light irradiates2Nano-tube array its static contact angle of water in the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane is less than 10 °, it is achieved that by the super-hydrophobic function to super hydrophilic transformation under different oil phase complex environments, as shown in Figure 5.
In this step, under above-mentioned oil phase, the water using pH to be 0 ~ 14 measures its static contact angle again smaller than 10 °, TiO2Nano-tube array the most also has ultra-hydrophobicity, embody its by super-hydrophobic acid-proof alkaline in super hydrophilic transition process, as shown in Figure 6.
Four, the TiO after above-mentioned steps three ultraviolet light being irradiated2 Nano-tube array, clean through deionized water rinsing equally, dry up, it is 150 DEG C in temperature, heats 1.5h, the static contact angle of water under normal hexane oil phase can be realized and be returned to again more than 150 °, there is again ultra-hydrophobicity, it is achieved that by the super hydrophilic function to super-hydrophobic reversible transition, as shown in Figure 4.
In this step, in addition to normal hexane, heated rear TiO2Nano-tube array its static contact angle of water in the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane is more than 150 °, it is achieved that by the super hydrophilic function to super-hydrophobic reversible transition in complex environment, as shown in Figure 5.
In this step, in above-mentioned oil phase, the water using pH to be 0 ~ 14 measures its static contact angle also greater than 150 °, embodies TiO2Nano-tube array is by super hydrophilic acid-proof alkaline during super-hydrophobic reversible transition, as shown in Figure 6.
In the present embodiment, TiO2Nano-tube array can realize at least 4 reversible transitions.
Embodiment
3
A kind of TiO2 nano-tube array specific embodiments with super-hydrophobic and super hydrophilic reversible transition function under oil is as follows:
One, the preparation of nano-metal-oxide array: using ammonium fluoride (0.3wt%) and ammonium sulfate mixed electrolytic solution, with metal leaf as anode, platinized platinum is negative electrode, and anodic oxidation voltage is 40V, and oxidization time is 2h, obtains WO3Nano-tube array.
Two, by the WO of preparation3Nano-tube array carries out heat treatment 1h at 350 DEG C, it is achieved that under normal hexane oil phase, the static contact angle of water is more than 150 °, has ultra-hydrophobicity, as shown in Figure 2.
In this step, in addition to normal hexane, thermally treated WO3Nanometer stick array static contact angle of water under the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane is all higher than 150 °, it is achieved also have ultra-hydrophobicity, as shown in Figure 5 under different oil phase complex environments.
Three, by WO after above-mentioned steps two heat treatment3Nano-tube array, clean through deionized water rinsing, dry up, 2h under ultraviolet light irradiates, under normal hexane oil phase, the static contact angle of water is less than 10 °, has super hydrophilicity, it is achieved that by the super-hydrophobic function to super hydrophilic transformation, as shown in Figure 3.
In this step, in addition to normal hexane, through the WO that ultraviolet light irradiates3Nano-tube array its static contact angle of water in the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane is less than 10 °, it is achieved that by the super-hydrophobic function to super hydrophilic transformation under different oil phase complex environments, as shown in Figure 5.
Four, the WO after above-mentioned steps three ultraviolet light being irradiated3Nano-tube array, clean through deionized water rinsing equally, dry up, it is 150 DEG C in temperature, heats 1.5h, the static contact angle of water under normal hexane oil phase can be realized and be returned to again more than 150 °, there is again ultra-hydrophobicity, it is achieved that by the super hydrophilic function to super-hydrophobic reversible transition, as shown in Figure 4.
In this step, in addition to normal hexane, heated rear WO3Nano-tube array its static contact angle of water in the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane is more than 150 °, it is achieved that by the super hydrophilic function to super-hydrophobic reversible transition in complex environment, as shown in Figure 5.
In the present embodiment, WO3Nano-tube array can realize at least 4 reversible transitions.
Embodiment
4
It is a kind of that to have the ZnO nano-rod array specific embodiments of super-hydrophobic and super hydrophilic reversible transition function under oil as follows:
One, the preparation of ZnO nano-rod array: take isopyknic 40mM/L hexamethylenetetramine and pin acid zinc respectively, temperature 65 DEG C is controlled after the mixing of 1:1, use electrochemical deposition method to deposit 800s under the conditions of the constant potential of-0.7V, obtain upright neat ZnO nano-rod array.
Two, the ZnO nano array of preparation is carried out heat treatment 1h at 350 DEG C, it is achieved that under normal hexane oil phase, the static contact angle of water is more than 150 °, has ultra-hydrophobicity.
In this step, in addition to normal hexane, thermally treated ZnO nano-rod array static contact angle of water under the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane is all higher than 150 °, it is achieved also have ultra-hydrophobicity under different oil phase complex environments.
Three, by the ZnO nano-rod array after step 2 heat treatment, clean through deionized water rinsing, dry up, 2h under ultraviolet light irradiates, under normal hexane oil phase, the static contact angle of water is less than 10 °, has super hydrophilicity, it is achieved that by the super-hydrophobic function to super hydrophilic transformation.
In this step, in addition to normal hexane, ZnO nano-rod array its static contact angle of water in the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane irradiated through ultraviolet light is less than 10 °, it is achieved that by the super-hydrophobic function to super hydrophilic transformation under different oil phase complex environments.
Four, the ZnO nano-rod array after step 3 ultraviolet light being irradiated, same clean through deionized water rinsing, dry up, it it is 130 DEG C in temperature, heating 2h, the static contact angle of water under normal hexane oil phase can be realized and be returned to again more than 150 °, there is again ultra-hydrophobicity, it is achieved that by the super hydrophilic function to super-hydrophobic reversible transition.
In this step, in addition to normal hexane, heated rear ZnO nano-rod array its static contact angle of water in the oil phases such as toluene, benzene, petroleum ether, hexamethylene, diesel oil and normal heptane is more than 150 °, it is achieved that by the super hydrophilic function to super-hydrophobic reversible transition in complex environment.
In the present embodiment, ZnO nano-rod array can realize at least 4 reversible transitions.
Claims (10)
1. one kind has the nano-metal-oxide array of super-hydrophobic and super hydrophilic reversible transition function under oil, after it is characterized in that described nano-metal-oxide array carries out heat treatment 1 ~ 4h at 120 ~ 350 DEG C, under oil phase, static contact angle is more than 150 °, has ultra-hydrophobicity;Under ultraviolet light irradiates after 1 ~ 2h, under oil phase, the static contact angle of water is less than 10 °, has super hydrophilicity, it is achieved by super-hydrophobic to super hydrophilic transformation;After heating reply 1.5 ~ 3h under the conditions of temperature is 100 ~ 150 DEG C, under oil phase, the static contact angle of water is returned to more than 150 °, has ultra-hydrophobicity, it is achieved by super hydrophilic to super-hydrophobic reversible transition.
The most according to claim 1 have the nano-metal-oxide array of super-hydrophobic and super hydrophilic reversible transition function under oil, it is characterised in that described nano-metal-oxide array is TiO2Nano-tube array, WO3Nano-tube array or ZnO nano-rod array.
The most according to claim 1 have the nano-metal-oxide array of super-hydrophobic and super hydrophilic reversible transition function under oil, it is characterised in that described oil phase is normal hexane, toluene, benzene, petroleum ether, hexamethylene, diesel oil or normal heptane.
The most according to claim 1 have the nano-metal-oxide array of super-hydrophobic and super hydrophilic reversible transition function under oil, it is characterised in that the number of times of described reversible transition is at least 4 times.
5. described in a claim 1, there is the preparation method of the nano-metal-oxide array of super-hydrophobic and super hydrophilic reversible transition function under oil, it is characterised in that described preparation method comprises the steps:
One, nano-metal-oxide array is carried out heat treatment so that it is under oil phase, there is ultra-hydrophobicity;
Two, by the nano-metal-oxide array after step one heat treatment, clean through deionized water rinsing, dry up, under ultraviolet light irradiates so that it is under oil phase, there is super hydrophilicity, it is achieved by the super-hydrophobic function to super hydrophilic transformation;
Three, the nano-metal-oxide array after step 2 ultraviolet light being irradiated, clean through deionized water rinsing equally, dry up, heating is replied so that it is have ultra-hydrophobicity under oil phase, it is achieved by the super hydrophilic function to super-hydrophobic reversible transition.
The most according to claim 5 have the preparation method of the nano-metal-oxide array of super-hydrophobic and super hydrophilic reversible transition function under oil, it is characterised in that described nano-metal-oxide array is TiO2Nano-tube array, WO3Nano-tube array or ZnO nano-rod array.
The most according to claim 6 have the preparation method of the nano-metal-oxide array of super-hydrophobic and super hydrophilic reversible transition function under oil, it is characterised in that described TiO2Nano-tube array and WO3Nano-tube array uses anodizing to prepare, and ZnO nano-rod array uses electrochemical deposition method to prepare.
The most according to claim 5 have the preparation method of the nano-metal-oxide array of super-hydrophobic and super hydrophilic reversible transition function under oil, it is characterised in that described oil phase is normal hexane, toluene, benzene, petroleum ether, hexamethylene, diesel oil or normal heptane.
The most according to claim 5 have the preparation method of the nano-metal-oxide array of super-hydrophobic and super hydrophilic reversible transition function under oil, it is characterised in that described preparation method also comprises the steps:
Five, repeat step three and four, carry out repeatedly reversible transition.
The most according to claim 9 have the preparation method of the nano-metal-oxide array of super-hydrophobic and super hydrophilic reversible transition function under oil, it is characterised in that the number of times of described repeatedly reversible transition is at least 4 times.
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