CN1663693A - Method for preparing super-amphiphobic micro-nano film on metal surface - Google Patents
Method for preparing super-amphiphobic micro-nano film on metal surface Download PDFInfo
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- CN1663693A CN1663693A CN 200510065816 CN200510065816A CN1663693A CN 1663693 A CN1663693 A CN 1663693A CN 200510065816 CN200510065816 CN 200510065816 CN 200510065816 A CN200510065816 A CN 200510065816A CN 1663693 A CN1663693 A CN 1663693A
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Abstract
The invention discloses a preparation method of super-double micro-nanometer film on metal surface, and relates to the treatment method of metal surface. The processes of the method are: prepare nanometer TiO2 film on the metal surface; carry out micro-nanometer treatment on the TiO2 film. The technique is simple and the feasibility is strong. The micro-nanometer treatment can maintain the thickness of the film and diminish the craze of the nanometer film. The invention only needs changing the temperature and the time to prepare the surface films with different shapes, and is not influenced by the kind, the shape and the size of the basic body. The surface F silicon alkyl treatment can prepare super-double nanometer TiO2 film and the erosion resistance is advanced by three quantity grades.
Description
Technical field
The present invention relates to a kind of processing method of metal surface, especially relate to a kind of in the super two methods of dredging micro-nano film of most of common metal surface constructions.
Background technology
No matter be basic research or aspect practical application, surface of solids wellability all causes people's extensive interest and attention, material surface super two dredge or super parents' characteristic has the important use meaning in a lot of high-tech areas.Because solution is the key factor that causes metal material generation electrochemical corrosion to destroy, surface wettability can become a key factor of control material corrosion again.Construct super two nano thin-film of dredging (hydrophobic oleophobic) performances in the metal surface, be expected to realize anticorrosion and automatically cleaning dual-use function metal.For the development of super two thin type nanometer film, at people (Tadanaga K.Katata N.Minami T., Super～water～repellent Al such as Japanese Tadanaga in 1997
2O
3Coating films with high transparency, J.Am.Ceram Soc., 1997,80:1040～1042) reported that employing sol～gel method and hydro-thermal post-processing technology have prepared boehmite (AlOOH) super-hydrophobic film with " Flower " pattern; (Nakajima A.Fujishima A.Hashimoto K. such as Nakajima, Preparation of transparent superhydrophobic boehmite and silica film bysublimation of Aluminum acetylacetonate, Adv.Mater., 1999,11 (6): 1365～1368).Adopt heating sublimation Al (C in the sintering process
5H
7O
2)
3Surface roughening boehmite or SiO
2The surface and subsequently silicon fluorideization prepare transparent nanometer film, and the windshield that is applied to automobile window glass has been obtained effect preferably.Construct the micro-nano TiO of super two thin types in the metal surface
2Film, can have " triple function " for the anticorrosion technique of material: hydrophobic effect, barrier effect and photoproduction cathodic protection effect have important actual application prospect.Correlative study does not appear in the newspapers as yet.
Summary of the invention
The present invention aims to provide a kind of in the super two methods of dredging micro-nano film of metal surface preparation.
In the super two methods of dredging micro-nano film of metal surface preparation, its step is
1) prepares the nano TiO 2 film in the metal surface;
2) on the nano TiO 2 film of metal surface, carry out micro-nanoization processing.
The said nano TiO 2 film for preparing in the metal surface adopts colloidal sol～gel method, at room temperature, after 10～50mL absolute ethyl alcohol and 1～5mL ethyl acetoacetate (EAcAc) mixing, adding 1～10ml butyl titanate reacts, the size that adds entry adjusting micelle leaves standstill aging to obtaining faint yellow transparent TiO2 colloidal sol.With metal use successively that acetone, absolute ethyl alcohol, three water are ultrasonic, cleaning, drying, metallic matrix is immersed in TiO2 colloidal sol, lift with the speed of 0.1～10mm/s, after the air dry, put under the infrared lamp dry.Again be immersed in the TiO2 colloidal sol, pulling film forming is used the infrared lamp drying again, and such preparation manipulation process repeats 3～4 times, and 450 ℃ of constant temperature calcination 10～60min reduce to room temperature more naturally.
The said water yield that adds the entry adjusting is 1～10mL.The frequency of three ultrasonic employings of water is 40kHz, and power is 80W, and the time is 10～30min.
Said method of carrying out micro-nanoization processing on metal-surface nano TiO2 film is that the metal sample of surface finish nano TiO2 film (being nano TiO 2 film/metal) is put into three water of 40～100 ℃, behind hydrothermal treatment consists 1～10h, air dry, at 100～600 ℃ of calcination 10～60min, naturally cooling, nanometer film/metal after micro-nanoization is put into the alcoholic solution of 0.1～5% silicon fluoride (FSA), take out after soaking 5～60min, dry under 100～200 ℃, promptly prepared super-hydrophobic type nano TiO 2 film/metal (SA/TiO2/316L).
The advantage that adopts the present invention can prepare the TiO2 film of super two thin type micro nano structures is, technology is simple, workable, equipment needed thereby is simple and easy, practical.Adopt the hydro-thermal post processing to nano TiO 2 film surface micronanoization, can keep under the constant condition of thickness, eliminate the be full of cracks in the nanometer film, solved with other technology and prepared the difficult problem that be full of cracks takes place nanometer film, especially only need the simple surface film that temperature and time just can prepare the different-shape structure that changes, be not subjected to the influence of factors such as matrix kind, shape, size simultaneously.Can prepare the micro nano structure TiO2 film of super two thin types through the processing of surperficial silicon fluoride base, can make the corrosion resistance of metal improve nearly 3 orders of magnitude, promptly the corrosion resistance of metal increases substantially.
Description of drawings
Fig. 1 is the SEM photo of nano TiO 2 film before the micro-nano technical finesse.
Fig. 2 is an AFM pattern (10 μ m * 10 μ m) of handling 1h rear surface TiO2 film through micro-nanoization technology (80 ℃).
Fig. 3 is an AFM pattern (10 μ m * 10 μ m) of handling 4h rear surface TiO2 film through micro-nanoization technology (80 ℃).
Fig. 4 is an AFM pattern (10 μ m * 10 μ m) of handling 4h rear surface TiO2 film through micro-nanoization technology (100 ℃).
Fig. 5 is the XRD spectrum of TiO2 after micro-nanoization processing.In Fig. 5, abscissa is 2 θ/deg, and ordinate is Intensity.(providing horizontal stroke, vertical target Chinese)
Fig. 6 is for forming the contact angle photo of super two thin types through the TiO2 of micro-nanoization processing film surface.
Fig. 7 is 316L stainless steel and the ac impedance spectroscopy of membrane electrode in 0.5mol/L NaCl solution, a) 316L; B) TiO2/316L; C) FSA/TiO2/316L.Fig. 7 (upward being Bode figure) a, b, c abscissa are that log frequency (H), ordinate (right side) are phase place (degree) for log impedance (Ω), ordinate (left side); Fig. 7 (being Nyqiust figure down) a, b, c, abscissa are impedance real part (M Ω), ordinate is imaginary impedance (M Ω))
Fig. 8 AC impedance analog circuit equivalent circuit, a) 316L stainless steel; (b) membrane electrode.
The specific embodiment
Following examples will the invention will be further described in conjunction with the accompanying drawings.
Embodiment 1
Under normal temperature, normal pressure, add 1ml EAcAc earlier in the 20ml absolute ethyl alcohol, under agitation add the 4ml butyl titanate, behind the reaction 1h, in 30min, add 0.2ml water, stir 5h, wait to film.The metallic matrix that preliminary treatment (surperficial machine glazed finish, the clean processing) is crossed is immersed in 5min in the colloidal sol, with at the uniform velocity lifting of 0.5mm/s, forms biofilm in the metal surface.Can see after the air dry that there is the nano TiO 2 film of one deck colour the metal surface, behind the dry 30min, repeat said process 3 times under the infrared lamp, put into 450 ℃ of calcination 30min of Muffle furnace constant temperature, natural cooling can make the nano TiO 2 film.Observe the nanometer film surface topography as shown in Figure 1 down at high power electronic scanner microscope (SEM), film is a porous membrane as seen from Figure 1, the surface is smooth substantially in order, the about 5nm of the diameter in hole, uniform particles distributes, a spot of particle agglomeration is arranged, and particle diameter is 18～20nm, and many particles have 3～4 granules reunions to form.
Test used medicine and be and analyze purely, adopt the pattern and the surface roughness of the U.S.'s NANOSCOPE IIIa of DI company scanning probe microscopy (SPM) test membrane; Adopt the elliptical polarization thickness tester of Shanghai University of Science and Technology to carry out the measurement of thickness.Adopt the Panalytical X ' pert of Philips company to change the particle crystal formation that target X～ray powder diffraction instrument is tested the nano TiO 2 film, test parameter is: CuK α target, λ is 0.15406nm, electric current 20mA, voltage 40kV, slit system is 1 ° of DS-1 ° of SS-0.15mmRS, with graphite monochromator filtering, and 1～4 °/min of sweep speed; Adopt the wellability on JC2000A contact angle measurement (go up marine morning company) test nanometer film surface, cyclohexane replaces oil, and the drop size is 5 μ L.Use the PGSTAT30 electrochemical workstation test decay resistance of Dutch Autolab company.
Utilize the corrosion-resistant behavior of electrochemical method test metal to have advantages such as simple, reliable.The present invention mainly adopts electrochemistry Tafel polarization method and electrochemical AC impedance method test surfaces to have the anticorrosive behavior after surface treatment of the 316L stainless steel base of super two thin type nanometer film.Three-electrode system is adopted in test, (area is that 1cm * 1cm) is a working electrode with membrane electrode, Pt is as auxiliary electrode, reference electrode is saturated calomel electrode (SCE), electrolyte is 0.5mol/L NaCl, and the whole test process electrolytic cell all is placed in the shielded box to reduce the interference of electromagnetism to test macro.
The nano TiO 2 film carry out surface micronanoization, earlier the nano TiO 2 film is put into 80 ℃ of three water, constant temperature is handled 1～10h, and is dry down at 200 ℃ after taking out.Fig. 2 is the surface topography of nanometer film behind the hydrothermal treatment consists 1h, as seen from Figure 2, the hole of micro-meter scale occurs on nano TiO 2 film surface, and the interface between the particle is clear, and the about 40nm of particle diameter has aggregation phenomenon, and the surface micronano secondary structure is obvious.As increase the hydrothermal treatment consists time to 4h, and the crosslinked micro-nano secondary structure of multi-layer net shape appears in the pattern (as Fig. 3) of nano surface TiO2 film, and mesh walls is smooth-out, and nano particle is fuzzy.
Embodiment 2
Adopt present technique to nano TiO 2 film surface micronanoization, can be by changing the pattern of temperature and time with the control nanometer film.Be placed in three water (pH=7) the nano TiO 2 film is outstanding equally, behind 100 ℃ of hydrothermal treatment consists 3h of constant temperature, it is dry down at 200 ℃ to take out the back.Fig. 4 is the surface topography at 100 ℃ of following hydrothermal treatment consists 3h nano TiO 2 films, and the visible surface pattern is the style type structure that is evenly distributed.Adopt XRD to characterize the crystal formation (Fig. 5) of particle in the nanometer film of micro-nanoization surface treatment front and back, the film of surface micronano structure mainly is TiO2 anatase (101), (004), (200), (211), (204), (220) and feature crystal faces such as (215) as can be seen from Figure 5, illustrates that the nanometer film of this method preparation does not influence the TiO2 crystal formation.
Embodiment 3
To the micro-nano film surface-assembled FSA behind the hydrothermal treatment consists 3h among the embodiment 1,2, the alcohol solution for soaking 1h that puts into 1% FSA takes out, and prepares hydrophobic type micro nano structure TiO2 film/316L at 170 ℃ of dry 1h, tests its surface wettability, and the result as shown in Figure 6.Can know its surface to the contact angle of water and cyclohexane all at 156 ± 1 °, prove that the film of surface micronano structure has tangible ultra-hydrophobicity.
Super two hydrophobic type micro nano structure TiO2 film/316L stainless steel corrosion resisting property characterizes.The preparation of the micro-nano TiO2 film of hydrophobic type/316L electrode as previously mentioned, electro-chemical test adopts three-electrode system, with the micro-nano TiO2 film of 316L, nano TiO 2 film and hydrophobic type/316l electrode as working electrode, the Pt plate electrode is as auxiliary electrode, reference electrode is saturated calomel electrode (SCE), and electrolyte is 0.5mol/L NaCl (pH=4.6) solution.AC impedence method is tested the corrosion resistance of different electrodes in NaCl solution, and test condition is with respect to OCP, and disturbance voltage is 10mV, and frequency range is 105～10～3Hz.Fig. 7 is the 316L stainless steel, TiO2/316L and the ac impedance spectroscopy of super two thin type nano TiO 2 membrane electrodes in 0.5mol/LNaCl solution, and wherein dotted line is an experimental data, solid line is a fitting data.Relatively three's Nyquist schemes, the erosion-resisting as can be known micro-nano TiO2 membrane electrode of super-hydrophobic type, nano TiO 2 membrane electrode and the 316L stainless steel electrode of being followed successively by from big to small, and the former has the poor of nearly 1～2 order of magnitude than the latter.Can see from Bode figure, behind the stainless steel surface nano film, two time parameters have appearred in its ac impedance spectroscopy, this is the characteristic properties of surface coverage film, its interfacial structure can be described with AC impedance equivalent circuit as shown in Figure 8, (a) be the stainless equivalent circuit of 316L, Rs is a solution resistance, and Rt and Qdl are interfacial reaction resistance and electric double layer capacitance; (b) be the equivalent circuit of membrane electrode, except above-mentioned parameter, have more (RQ) constant of a pair of description film character, be respectively film resistance Rc and electric capacity Qc.By match to equivalent circuit, can obtain the numerical value of above-mentioned each element of equivalent circuit, as shown in table 1.The result shows equally, the electrochemical reaction resistance ratio stainless steel electrode of super-hydrophobic type nanometer film electrode has increased 3 orders of magnitude, compare with the nano TiO 2 membrane electrode, electrochemical reaction resistance increases nearly 2 orders of magnitude, shows that the TiO2 film of the micro nano structure of super-hydrophobic type has better Corrosion Protection than conventional TiO2 membrane electrode.
Table 1 AC impedance equivalent circuit fitting parameter
| ????No | ??R s?Ω.cm 2 | ??????????????Q dl | ??R cΩ.cm 2 | ???????????????Q dl | ????R t??Ω.cm 2 | ||
| ????Y 0??Ω ～1.cm ～2????.s ～n | ????n | ????Y 0??Ω ～1.cm ～2????.s ～n | ????n | ||||
| ?316L | ??30.9 | ????～ | ??～ | ???～ | ??6.08×10 ～6 | ?0.9 | ??1.32×10 5 |
| ?TiO 2/316L | ??45.8 | ??4.4×10 ～8 | ??0.7 | ??2152 | ??1.90×10 ～6 | ?0.9 | ??1.68×10 6 |
| ?FAS/TiO 2/316L | ??38.0 | ??1.6×10 ～9 | ??0.6 | ??884 | ??1.54×10 ～6 | ?0.9 | ??2.03×10 8 |
Claims (5)
1, a kind of method for preparing super-amphiphobic micro-nano film on metal surface is characterized in that its step is
1) prepares the nano TiO 2 film in the metal surface;
2) on the nano TiO 2 film of metal surface, carry out micro-nanoization processing.
2, a kind of method for preparing super-amphiphobic micro-nano film on metal surface as claimed in claim 1, it is characterized in that the said nano TiO 2 film for preparing in the metal surface adopts colloidal sol～gel method, at room temperature, after 10～50mL absolute ethyl alcohol and the mixing of 1～5mL ethyl acetoacetate, adding 1～10ml butyl titanate reacts, add entry and regulate the size of micelle to obtaining faint yellow transparent TiO2 colloidal sol, leave standstill aging, metal is used acetone successively, absolute ethyl alcohol, three times water is ultrasonic, clean, drying is immersed in TiO2 colloidal sol to metallic matrix, lifts with the speed of 0.1～10mm/s, after the air dry, put into drying under the infrared lamp, be immersed in the TiO2 colloidal sol pulling film forming more again, use the infrared lamp drying, repeat 3～4 times, 450 ℃ of constant temperature calcination 10～60min reduce to room temperature more naturally.
3, a kind of method for preparing super-amphiphobic micro-nano film on metal surface as claimed in claim 2 is characterized in that the said water yield that adds the entry adjusting is 1～10mL.
4, a kind of method for preparing super-amphiphobic micro-nano film on metal surface as claimed in claim 2, the frequency that it is characterized in that three ultrasonic employings of water is 40kHz, and power is 80W, and the time is 10～30min.
5, a kind of method for preparing super-amphiphobic micro-nano film on metal surface as claimed in claim 1, it is characterized in that said method of carrying out micro-nanoization processing on metal-surface nano TiO2 film is the metal sample of surface finish nano TiO2 film to be put into three water of 40～100 ℃, behind hydrothermal treatment consists 1～10h, air dry, at 100～600 ℃ of calcination 10～60min, naturally cooling, nanometer film/metal after micro-nanoization is put into the alcoholic solution of 0.1～5% silicon fluoride, take out after soaking 5～60min, dry under 100～200 ℃, promptly prepared super-hydrophobic type nano TiO 2 film/metal.
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| CN102380230A (en) * | 2011-09-05 | 2012-03-21 | 北京航空航天大学 | Hierarchical micro-nanostructure omentum based light-operated oil-water separator and its application method |
| CN102553813A (en) * | 2012-02-17 | 2012-07-11 | 天津大学 | Sol-gel method for preparing micro/nano titanium dioxide and lyophobic film thereof on metal surfaces |
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| CN106903035A (en) * | 2015-12-22 | 2017-06-30 | 北京奥托米特电子有限公司 | Corrosion resistance structure and preparation method thereof |
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| CN107058985A (en) * | 2017-05-05 | 2017-08-18 | 孝感双华应用科技开发有限公司 | A kind of preparation method of titanium dioxide hydrophobic membrane |
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| CN102380230A (en) * | 2011-09-05 | 2012-03-21 | 北京航空航天大学 | Hierarchical micro-nanostructure omentum based light-operated oil-water separator and its application method |
| CN102380230B (en) * | 2011-09-05 | 2013-07-24 | 北京航空航天大学 | Hierarchical micro-nanostructure omentum based light-operated oil-water separator and its application method |
| CN102310038A (en) * | 2011-09-29 | 2012-01-11 | 华东交通大学 | Method for improving surface hydrophobicity of metal film |
| CN102553813A (en) * | 2012-02-17 | 2012-07-11 | 天津大学 | Sol-gel method for preparing micro/nano titanium dioxide and lyophobic film thereof on metal surfaces |
| CN102553813B (en) * | 2012-02-17 | 2013-10-30 | 天津大学 | Sol-gel method for preparing micro/nano titanium dioxide and lyophobic film thereof on metal surfaces |
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| CN104176774A (en) * | 2014-07-24 | 2014-12-03 | 西安理工大学 | Preparation method of titanium dioxide superhydrophobic film |
| CN104176774B (en) * | 2014-07-24 | 2016-02-24 | 西安理工大学 | A kind of preparation method of titanium dioxide based superhydrophobic thin films |
| WO2016082153A1 (en) * | 2014-11-27 | 2016-06-02 | Honeywell International Inc. | Omniphobic coating |
| US10590285B2 (en) | 2014-11-27 | 2020-03-17 | Honeywell International Inc. | Omniphobic coating |
| CN106903035A (en) * | 2015-12-22 | 2017-06-30 | 北京奥托米特电子有限公司 | Corrosion resistance structure and preparation method thereof |
| CN106917087A (en) * | 2017-04-17 | 2017-07-04 | 东南大学 | One kind has steel bar anti-corrosion, the preparation method of hydrophobic double effects diaphragm |
| CN107058985A (en) * | 2017-05-05 | 2017-08-18 | 孝感双华应用科技开发有限公司 | A kind of preparation method of titanium dioxide hydrophobic membrane |
| CN107058985B (en) * | 2017-05-05 | 2018-12-04 | 绍兴泽美纺织品有限公司 | A kind of preparation method of titanium dioxide hydrophobic membrane |
| CN108466015A (en) * | 2018-04-10 | 2018-08-31 | 清华大学 | A kind of super-amphiphobic metal surface and preparation method thereof of nanostructure distributed in three dimensions |
| CN111266277A (en) * | 2020-02-21 | 2020-06-12 | 福建师范大学 | Lubricating fluid injection type super-smooth silicone rubber/nano inorganic matter dynamic hydrophobic-oleophobic hybrid coating and construction method and application thereof |
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