CN106283151A - A kind of preparation method of wear-resisting based superhydrophobic thin films - Google Patents
A kind of preparation method of wear-resisting based superhydrophobic thin films Download PDFInfo
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- CN106283151A CN106283151A CN201610782333.3A CN201610782333A CN106283151A CN 106283151 A CN106283151 A CN 106283151A CN 201610782333 A CN201610782333 A CN 201610782333A CN 106283151 A CN106283151 A CN 106283151A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses the preparation method of a kind of wear-resisting based superhydrophobic thin films, first passing through electro-deposition techniques, to prepare one layer of mechanical strength height, adhesion on metallic matrix good, and has the SiO of high porosity2Thin film, then by electrophoretic techniques, the super-hydrophobicity Nano-meter SiO_2 will modified through surface2Powder is filled in above-mentioned SiO2In the duct of thin film, thus prepare the based superhydrophobic thin films with excellent wear-resisting property.Described super-hydrophobicity Nano-meter SiO_22Powder is by nanoscale SiO2The hydrophobic silane such as powder and long chain organic silanes such as dodecyltrimethoxysilane, hexadecyl trimethoxy silane, octadecyl trimethoxysilane or chloride, fluorine, such as octadecyl trichlorosilane alkane, perfluoro capryl trimethoxy silane etc., graft modification is occurred to prepare in the basic conditions.The above-mentioned method preparing based superhydrophobic thin films that the present invention provides is simple to operate, cost is relatively low, mild condition, is expected to large-scale application in industrialized production.
Description
Technical field
The present invention relates to the gentle preparation of wear-resisting based superhydrophobic thin films, particularly relate to a kind of wear-resisting super-hydrophobic silica thin film
Preparation method.
Background technology
Super hydrophobic material, refers to that contact angle is more than 150 °, the roll angle a kind of special material less than 10 °.In recent years, utilize
Its special " not getting wet " characteristic, super hydrophobic material is used widely at a lot of aspects, as self-cleaning surface, surface are prevented
Freeze, the field such as metal protection.But, there is mechanical performance not in the superhydrophobic thin film material majority using conventional method to prepare gained
The shortcomings such as good, wearability is bad, largely limit its actual application.
Be there is the super hydrophobic surface of good abrasion resistance at present by two kinds of basic skills preparations.One is to use flexible material
(such as fabric, Cotton Gossypii etc.) be remarkably improved as matrix the super hydrophobic surface of its surface construction anti-wear performance (Adv.Mater.,
2012,24,2409.)；Two is to use the thinning method of etching to prepare at hard material surface to have identical with matrix material
The super hydrophobic surface (J.Mater.Chem.A, 2016,4,3406) of anti-wear performance.But, above-mentioned first method exists heat-resisting
The shortcoming of limited capacity, matrix, owing to being that one damages technology, is damaged by second method.
Summary of the invention
The present invention is directed to the problems referred to above present in the preparation of previous wearability super hydrophobic surface, propose high with mechanical strength,
Adhesion is good, and has the electro-deposition SiO of high porosity2Thin film is matrix skeleton, and then will be super thin by electrophoretic techniques
The Nano-meter SiO_2 of water2Powder is filled in above-mentioned firm skeleton dispersedly, prepares novel wear resistant super hydrophobic surface.
Realize by following technical solution:
The preparation method of a kind of wear-resisting based superhydrophobic thin films, comprises the following steps:
1) metallic matrix is after sand papering to 600 mesh, after the most ultrasonic 10 minutes take out, through tap water, go from
60 DEG C of thermostatic drying chambers are put into stand-by after sub-water cleaning, drying；
2) ethanol 50mL, 0.2M NaNO are measured350mL, after mixing, adds tetraethyl orthosilicate 5mL, and the pH of solution adjusts
Joint is 4.5, standby after magnetic agitation 12h.
3) use three-electrode system good in one layer of mechanical strength height of metallic matrix substrates, adhesion, and there is height
The SiO of loose structure2Thin film, wherein working electrode is metallic matrix, and Pt sheet, Ag/AgCl (saturated KCl) electrode are respectively as right
Electrode and reference electrode, the current potential of applying is-1.0V～-2.0V, and electrodeposition time is 200～600s.
3) 2g nanoscale SiO is weighed2Powder is dispersed in the ammonia spirit of 100mL pH=8, standby after magnetic agitation 1h；
In another container, add 5mL hydrophobicity long chain silane be dispersed in 100mL ethanol, standby after magnetic agitation 1h, by rear one molten
Liquid is added dropwise in previous solution, and magnetic agitation forms homogeneous suspension after 6 hours, after being aged 4 hours, and centrifugation,
The white powder obtained is dried in 60 DEG C of baking ovens, obtains super-hydrophobic SiO2Powder；
4) the super-hydrophobic SiO that mass fraction is 0.1%～10% is weighed2Powder is distributed in non-polar organic solvent, super
After sound dispersion 10min, obtain electrophoresis liquid；
5) on DC source, two electrode systems are used to carry out electrophoretic deposition in electrophoresis liquid, to cover electro-deposition
SiO2The metallic matrix of thin film is as positive pole, and Pt electrode is as negative pole, and two electrode spacings 35mm, Control of Voltage is 5～80V, electric
The swimming time controls, 1～10min, after electrophoresis terminates, sample to be placed in the drying in oven of 60 DEG C, obtains based superhydrophobic thin films.
In technique scheme, described metallic matrix include galvanized steel, aluminum, magnesium, titanium, rustless steel, mild steel or other
Conducting metal and alloy.
The described hydrophobicity long chain silane being used for preparing super-hydrophobic nano SiO 2 powder includes dodecyl front three
The hydrophobic silane such as TMOS, hexadecyl trimethoxy silane, octadecyl trimethoxysilane or chloride, fluorine, such as ten
Eight alkyltrichlorosilanes, perfluoro capryl trimethoxy silane etc..
The solvent of described electrophoresis solution is normal hexane, hexadecane or other non-polar organic solvents.
Advantages of the present invention and beneficial effect: (1) silica based materials numerous using resource, eco-friendly is as former
Material；(2) the electro-deposition SiO that mechanical strength is high, adhesion is strong, porous is high is used2Thin film is as matrix skeleton, it is ensured that wearability
Energy；(3) electrophoretic techniques is used to be filled into dispersed for super-hydrophobic silica powder in whole stephanoporate framework, it is ensured that different mills
Damage the ultra-hydrophobicity under the degree of depth；Meanwhile, electrophoresis method has that resource utilization is high and the advantage such as technique is simple；(4) due to compound
Thin film is formed by inorganic oxide, has good heat resistance simultaneously；(5) the inventive method is simple to operate, reproducible,
Material cost is relatively low, low to facility requirements, is expected to heavy industrialization application.
Accompanying drawing explanation
Fig. 1 (a) electro-deposition SiO2The optical photograph of thin film and contact angle photo (matrix is aluminium alloy AA2024-T3) thereof；
B () is with electro-deposition SiO2Thin film is matrix, and then the SiO that electrophoretic deposition is super-hydrophobic2Optical photograph after powder and
Contact angle photo (metallic matrix is aluminium alloy AA2024-T3).
Fig. 2 is with naked aluminium alloy (1) and electro-deposition in advance SiO2The aluminium alloy of thin film (2) is matrix, and then electrophoretic deposition
Super-hydrophobic SiO2Wearability test result (pressure: the 0.6kPa of the based superhydrophobic thin films obtained after powder；Sand paper mesh number: 1200；
The friction length of each circulation: 16cm).
Detailed description of the invention
The preparation method of a kind of wear-resisting based superhydrophobic thin films, comprises the following steps:
1) metallic matrix is after sand papering to 600 mesh, after the most ultrasonic 10 minutes take out, through tap water, go from
60 DEG C of thermostatic drying chambers are put into stand-by after sub-water cleaning, drying；
2) ethanol 50mL, 0.2M NaNO are measured350mL, after mixing, adds tetraethyl orthosilicate 5mL, and the pH of solution adjusts
Joint is about 4.5, standby after magnetic agitation 12h.
3) use three-electrode system good in one layer of mechanical strength height of metal substrates, adhesion, and have highly porous
The SiO of structure2Thin film, wherein working electrode is metallic matrix, and Pt sheet, Ag/AgCl (saturated KCl) electrode are respectively as to electrode
And reference electrode, the current potential of applying is-1.0V～-2.0V, and electrodeposition time is 200～600s.
3) 2g nanoscale SiO is weighed2Powder is dispersed in the ammonia spirit of 100mL pH=8, standby after magnetic agitation 1h；
In another container, add 5mL hydrophobicity long chain silane be dispersed in 100mL ethanol, standby after magnetic agitation 1h, by rear one molten
Liquid is added dropwise in previous solution, and magnetic agitation forms homogeneous suspension after 6 hours, after being aged 4 hours, and centrifugation,
The white powder obtained is dried in 60 DEG C of baking ovens, obtains super-hydrophobic SiO2Powder；
4) the super-hydrophobic SiO that mass fraction is 0.1%～10% is weighed2Powder is distributed in non-polar organic solvent, super
After sound dispersion 10min, obtain electrophoresis liquid；
5) on DC source, two electrode systems are used to carry out electrophoretic deposition in electrophoresis liquid, to cover electro-deposition
SiO2The metallic matrix of thin film is as positive pole, and Pt electrode is as negative pole, and two electrode spacings 35mm, Control of Voltage is 5～80V, electric
The swimming time controls, 1～10min, after electrophoresis terminates, sample to be placed in the drying in oven of 60 DEG C, obtains based superhydrophobic thin films.
Described metallic matrix includes galvanized steel, aluminum, magnesium, titanium, rustless steel, mild steel or other conducting metals and conjunction
Gold.The described long chain silane for preparing super-hydrophobic nano SiO 2 powder include dodecyltrimethoxysilane, ten
The hydrophobic silane such as six alkyl trimethoxysilanes, octadecyl trimethoxysilane or chloride, fluorine, such as octadecyl trichlorosilane
Alkane, perfluoro capryl trimethoxy silane etc..The solvent of described electrophoresis solution be normal hexane, hexadecane or other nonpolar have
Machine solvent.
Embodiment 1
Matrix uses commercial alloy matrix aluminum AA2024-T3, after sand papering to 600 mesh, the most ultrasonic 10
Take out after minute, after tap water, deionized water cleaning, drying, put into 60 DEG C of thermostatic drying chambers stand-by.
Hydrophobicity SiO2The preparation of powder:
Solution 1 forms: weigh 1g Nano-meter SiO_22Powder is dispersed in the solution of 100mL pH=8, wherein the control of pH value of solution
System is to use ammonia to be adjusted, standby after magnetic agitation 1h；Solution 2 forms: divided by the dodecyltrimethoxysilane of 5mL
It is dispersed in 100mL ethanol, standby after magnetic agitation 1h.Being added dropwise in solution 1 by above-mentioned solution 2, magnetic agitation is after 6 hours
Form homogeneous suspension, be aged 4 hours standby.After centrifugation, (rotating speed controls at 10000r/min, and disengaging time is
10min), after abandoning supernatant, it is dried in gained powder is placed in the air dry oven of 60 DEG C, finally gives super-hydrophobic
SiO2Powder is standby.
The preparation of electrophoresis solution: weigh the super-hydrophobic SiO of above-mentioned preparation2Powder is distributed in normal hexane, wherein SiO2Matter
Amount is divided into 0.1%, standby after ultrasonic disperse 10min.
Electro-deposition SiO2The preparation of precursor solution: measure ethanol 50mL, 0.2M NaNO350mL, after mixing, is just adding
Tetraethyl orthosilicate 5mL, the pH regulator of solution is about 4.5, standby after magnetic agitation 12h.
Electro-deposition SiO2The preparation of thin film: use three-electrode system at above-mentioned SiO2Precursor solution carries out electro-deposition, its
Middle alloy matrix aluminum is working electrode, and Pt sheet, Ag/AgCl (saturated KCl) electrode are respectively as to electrode and reference electrode, work
The current potential applied on electrode is-1.0V, and electrodeposition time is 600s.(the named Al-SiO of sample of preparation2)
The super-hydrophobic SiO of electrophoresis2The preparation of thin film: on DC source, in the electrophoresis solution of above-mentioned configuration, uses two electricity
Polar body system carries out electrophoretic deposition, with Al-SiO2As working electrode, Pt is as to electrode, between the two away from for 35mm, Control of Voltage
At 5V, electrophoresis time is 10min, after electrophoresis terminates, sample is placed in the drying in oven of 60 DEG C.
The SiO of electro-deposition gained2Thin film, shows Superhydrophilic, and through the super-hydrophobic nano silicon of follow-up electrophoresis
After powder, matrix presents super-hydrophobic state, as shown in Figure 1.In wearability test, by the metallographic on film sample surface Yu 1200 mesh
Sand paper contacts, and applies the pressure of 0.6kPa, draws sample with the speed of 10mm/s.Experimental result is as in figure 2 it is shown, legend 1,2 is distinguished
For naked aluminum alloy surface and Al-SiO2On surface, the contact angle after electrophoretic deposition super-hydrophobic silica powder is with Rubbing number
Variation relation (the most each circulation 16cm).Contrast test result is it is found that control sample is through less than a circulation (
Individual cycling distance is 16cm), thin film the most large-scale damage, matrix is become from original super-hydrophobic (contact angle is 155 °)
Hydrophilic (34.1 °)；And sample super-hydrophobic for the present invention, after 20 circulations, still keeping super-hydrophobic state.This explanation
Electro-deposition SiO2The introducing of thin-film carrier, significantly improves the anti-wear performance of electrophoresis based superhydrophobic thin films.
Embodiment 2
In the present embodiment, other steps are similar to Example 1, still with aluminium alloy as matrix, but electro-deposition SiO2Sinking of thin film
Long-pending current potential is-2.0V, and sedimentation time is 200s.Under above-mentioned process conditions, same can get can be born～the friction survey of 20 circulations
Examination, the contact angle of sample remains at about 159 °.
Embodiment 3
It is embodied as step similar to Example 1, changes hydrophobicity SiO in electrophoresis liquid2The concentration of nano-particle.Hydrophobicity
SiO2The concentration of nano-particle and final gained based superhydrophobic thin films contact angle and can to bear the relation of Rubbing number as shown in the table:
Hydrophobicity SiO in table 1 electrophoretic deposition liquid2Concentration and contact angle and concentration relationship
Embodiment 4
It is embodied as step similar to Example 1, super-hydrophobic SiO2Concentration is 0.1%, changes electrophoretic deposition liquid nonpolar
The kind of organic solvent, all can prepare wear-resisting based superhydrophobic thin films.
The impact of non-polar solven in table 2 electrophoretic deposition liquid
Embodiment 5
It is embodied as step similar to Example 1, but matrix uses titanium plate, one layer of SiO of electro-deposition in advance2Thin film, then
The super-hydrophobic SiO of electrophoretic deposition2Granule, gained meets surface after 50 rub cycle, and contact angle still can maintain 153.6 °.
Above-described embodiment be used for illustrate the present invention rather than limit the invention, the present invention spirit and
In scope of the claims, any modifications and changes that the present invention is made, both fall within the protection domain of invention.
Claims (4)
1. the preparation method of a wear-resisting based superhydrophobic thin films, it is characterised in that comprise the following steps:
1) metallic matrix is after sand papering to 600 mesh, takes out, through tap water, deionized water after the most ultrasonic 10 minutes
60 DEG C of thermostatic drying chambers are put into stand-by after cleaning, drying；
2) ethanol 50mL, 0.2M NaNO are measured350mL, after mixing, adds tetraethyl orthosilicate 5mL, and the pH regulator of solution exists
4.5, standby after magnetic agitation 12h.
3) use three-electrode system at the SiO of one layer of loose structure of metallic matrix substrates2Thin film, wherein working electrode is gold
Belong to matrix, Pt sheet, Ag/AgCl (saturated KCl) electrode respectively as to electrode and reference electrode, the current potential of applying be-1.0V～-
2.0V, electrodeposition time is 200～600s；
3) 2g nanoscale SiO is weighed2Powder is dispersed in the ammonia spirit of 100mL pH=8, standby after magnetic agitation 1h；Separately
In one container add 5mL hydrophobicity long chain silane be dispersed in 100mL ethanol, standby after magnetic agitation 1h, by a rear solution by
Being added dropwise in previous solution, magnetic agitation forms homogeneous suspension after 6 hours, after being aged 4 hours, and centrifugation, obtain
White powder in 60 DEG C of baking ovens be dried, obtain super-hydrophobic SiO2Powder；
4) the super-hydrophobic SiO that mass fraction is 0.1%～10% is weighed2Powder is distributed in non-polar organic solvent, ultrasonic disperse
After 10min, obtain electrophoresis liquid；
5) on DC source, two electrode systems are used to carry out electrophoretic deposition in electrophoresis liquid, to cover electro-deposition SiO2Thin film
Metallic matrix as positive pole, Pt electrode as negative pole, two electrode spacings 35mm, Control of Voltage 5～80V, electrophoresis time control
Sample, 1～10min, after electrophoresis terminates, is placed in the drying in oven of 60 DEG C, obtains based superhydrophobic thin films by system.
The preparation method of a kind of wear-resisting based superhydrophobic thin films the most according to claim 1, it is characterised in that described Metal Substrate
Body is galvanized steel, aluminum, magnesium, titanium, rustless steel, mild steel or other conducting metals and alloy.
The preparation method of a kind of wear-resisting based superhydrophobic thin films the most according to claim 1, it is characterised in that described being used for is made
The hydrophobicity long chain silane of standby super-hydrophobic nano SiO 2 powder is dodecyltrimethoxysilane, cetyl trimethoxy
The hydrophobic silane such as base silane, octadecyl trimethoxysilane or chloride, fluorine, such as octadecyl trichlorosilane alkane, perfluoro capryl
Trimethoxy silane etc..
The preparation method of a kind of wear-resisting based superhydrophobic thin films the most according to claim 1, it is characterised in that described electrophoresis is molten
The solvent of liquid is normal hexane, hexadecane or other non-polar organic solvents.
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Cited By (10)
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| CN107383949A (en) * | 2017-07-21 | 2017-11-24 | 南通天驰环保科技有限公司 | A kind of wear-resisting anti-reflection hydrophobic film coating liuqid of automatically cleaning photovoltaic glass and preparation method thereof |
| CN107641832A (en) * | 2017-09-19 | 2018-01-30 | 重庆大学 | A kind of preparation method of super-hydrophobic stainless (steel) wire nanometer aluminium film |
| CN107955959A (en) * | 2017-11-16 | 2018-04-24 | 中国科学院宁波材料技术与工程研究所 | The super-hydrophobic modifies SiO of aniline trimerization2Hybrid coating, its preparation method and application |
| CN108517551A (en) * | 2018-04-10 | 2018-09-11 | 浙江工业大学 | A kind of System of Silica/Aluminum Microparticle coating and its preparation process |
| CN109137045A (en) * | 2018-09-13 | 2019-01-04 | 湖北大学 | A method of colour super-hydrophobic stainless steel is prepared based on alkali electrochemical coloring |
| CN109821718A (en) * | 2019-02-14 | 2019-05-31 | 清华大学 | A kind of wear-resistant super lyophoby material and preparation method thereof |
| CN111054435A (en) * | 2019-12-30 | 2020-04-24 | 苏州东杏表面技术有限公司 | Novel supported Pt catalyst, preparation method thereof and application thereof in hydrogen silicon addition |
| CN111364122A (en) * | 2020-03-18 | 2020-07-03 | 浙江恒远化纤集团有限公司 | Porous PBT fiber POY (polyester pre-oriented yarn) and preparation method thereof |
| CN112094589A (en) * | 2020-09-21 | 2020-12-18 | 四川大学 | Preparation and application of environment-friendly low-cost super-hydrophobic powder material |
| CN113583543A (en) * | 2021-09-02 | 2021-11-02 | 苏州科技大学 | Preparation method and application of hydrophobic composite anti-corrosion coating |
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| CN107383949A (en) * | 2017-07-21 | 2017-11-24 | 南通天驰环保科技有限公司 | A kind of wear-resisting anti-reflection hydrophobic film coating liuqid of automatically cleaning photovoltaic glass and preparation method thereof |
| CN107641832A (en) * | 2017-09-19 | 2018-01-30 | 重庆大学 | A kind of preparation method of super-hydrophobic stainless (steel) wire nanometer aluminium film |
| CN107955959B (en) * | 2017-11-16 | 2019-08-16 | 中国科学院宁波材料技术与工程研究所 | The super-hydrophobic modifies SiO of aniline trimerization2Hybrid coating, its preparation method and application |
| CN107955959A (en) * | 2017-11-16 | 2018-04-24 | 中国科学院宁波材料技术与工程研究所 | The super-hydrophobic modifies SiO of aniline trimerization2Hybrid coating, its preparation method and application |
| CN108517551A (en) * | 2018-04-10 | 2018-09-11 | 浙江工业大学 | A kind of System of Silica/Aluminum Microparticle coating and its preparation process |
| CN109137045A (en) * | 2018-09-13 | 2019-01-04 | 湖北大学 | A method of colour super-hydrophobic stainless steel is prepared based on alkali electrochemical coloring |
| CN109137045B (en) * | 2018-09-13 | 2019-10-25 | 湖北大学 | A method of colour super-hydrophobic stainless steel is prepared based on alkali electrochemical coloring |
| CN109821718A (en) * | 2019-02-14 | 2019-05-31 | 清华大学 | A kind of wear-resistant super lyophoby material and preparation method thereof |
| CN111054435A (en) * | 2019-12-30 | 2020-04-24 | 苏州东杏表面技术有限公司 | Novel supported Pt catalyst, preparation method thereof and application thereof in hydrogen silicon addition |
| CN111054435B (en) * | 2019-12-30 | 2023-01-24 | 苏州东杏表面技术有限公司 | Novel supported Pt catalyst, preparation method thereof and application thereof in hydrogen silicon addition |
| CN111364122A (en) * | 2020-03-18 | 2020-07-03 | 浙江恒远化纤集团有限公司 | Porous PBT fiber POY (polyester pre-oriented yarn) and preparation method thereof |
| CN112094589A (en) * | 2020-09-21 | 2020-12-18 | 四川大学 | Preparation and application of environment-friendly low-cost super-hydrophobic powder material |
| CN112094589B (en) * | 2020-09-21 | 2021-12-14 | 四川大学 | Preparation and application of environment-friendly low-cost super-hydrophobic powder material |
| CN113583543A (en) * | 2021-09-02 | 2021-11-02 | 苏州科技大学 | Preparation method and application of hydrophobic composite anti-corrosion coating |
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