CN109628978A - A kind of preparation method of erosion resistant super hydrophobic surface - Google Patents
A kind of preparation method of erosion resistant super hydrophobic surface Download PDFInfo
- Publication number
- CN109628978A CN109628978A CN201910060768.0A CN201910060768A CN109628978A CN 109628978 A CN109628978 A CN 109628978A CN 201910060768 A CN201910060768 A CN 201910060768A CN 109628978 A CN109628978 A CN 109628978A
- Authority
- CN
- China
- Prior art keywords
- erosion resistant
- super hydrophobic
- preparation
- resistant super
- hydrophobic surface
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/24—Chemical after-treatment
Abstract
The present invention relates to Treatment of Metal Surface and modified fields, and in particular to a kind of preparation method of erosion resistant super hydrophobic surface.Substrate after surface treatment is subjected to constant pressure anodic oxidation in using oxalic acid aqueous solution as electrolyte solution, low-surface-energy molecular modification is carried out after oxidation, heat treatment can form erosion resistant super hydrophobic surface in substrate surface.The method of the present invention preparation process is simple, it is reproducible, low in cost, convenient for being widely applied, resulting super hydrophobic surface contact angle reaches 164.7 °, with excellent automatically cleaning, wear and corrosion resistance, have broad application prospects in marine corrosion and protection field.
Description
Technical field:
The present invention relates to Treatment of Metal Surface and modified fields, and in particular to a kind of preparation side of erosion resistant super hydrophobic surface
Method.
Background technique:
As a kind of special wetability state, super hydrophobic surface receives significant attention in recent years, surface solid-liquid-gas
Three phase boundary typical Cassie-Baxter model contact makes super hydrophobic material in self-cleaning surface, water-oil separating, antifog anti-
The fields such as ice, fluid drag-reduction, marine anticorrosion be antifouling are shown good application potential.The main side of super hydrophobic surface is prepared at present
Method is all based on the building and low-surface-energy modification of surface micro-nano structure mostly.
However, the microstructure on surface is highly susceptible to wear and destroy when super hydrophobic surface is by mechanical friction,
And then leading to the forfeiture of surface super hydrophobic characteristic, it is always to limit it in the big face in each field that super hydrophobic surface mechanical stability is not good enough
The critical issue that product promotes and applies, therefore the excellent super hydrophobic surface of wearability how is prepared, and there is important reality to anticipate
Justice.
Summary of the invention:
To solve the above problems, the present invention provides a kind of preparation methods of erosion resistant super hydrophobic surface.
To achieve the above object, the invention adopts a technical scheme as:
A kind of preparation method of erosion resistant super hydrophobic surface, by the substrate after surface treatment using oxalic acid aqueous solution as electricity
In electrolyte solution carry out constant pressure anodic oxidation, after oxidation carry out low-surface-energy molecular modification, heat treatment can be in substrate surface shape
At erosion resistant super hydrophobic surface.
The constant pressure anodic oxidation is that will be surface-treated rear substrate to be placed in bipolar electrode anodic oxidation system, water-soluble with oxalic acid
For liquid as electrolyte solution, substrate is anode, and platinum electrode is cathode, 35-50V voltage anodic oxygen 5-15min.
By sample substrate after the anodic oxidation, cleaned repeatedly respectively with deionized water and dehydrated alcohol.
The oxalic acid aqueous solution concentration is 0.2-0.4mol/L.
Further, oxidation rear substrate is immersed in 5- in the ethanol solution of perfluoro decyl triethoxysilane at room temperature
120min then takes out and heats 10-60min at 100-200 DEG C；The submergence generally in soaking at room temperature, is impregnated
Time 5-120min, so that the silicon fluoride molecule of one layered low-surface energy of substrate surface modification and covering.
The concentration of perfluoro decyl triethoxysilane is 1- in the ethanol solution of the perfluoro decyl triethoxysilane
3%.
The substrate surface carries out pre-treatment: sample is placed in dehydrated alcohol and deionized water is cleaned by ultrasonic first, with
Afterwards using the SiC sand paper polishing matrix of different meshes (200,400,800,1200,2000).
A kind of erosion resistant super-hydrophobic film forms erosion resistant super-hydrophobic film in substrate surface according to the method.
Above-mentioned substrate is aluminium alloy or rafifinal.
Compared with prior art, the invention has the following advantages:
(1) process of preparing of the present invention is simple, reproducible, using current widely used anodizing technology conduct
Construct the main means of micro-nano structure, it is low in cost, convenient for being widely applied.
(2) super hydrophobic surface that preparation method of the present invention obtains has low adhesive force and excellent automatically cleaning characteristic, and
Corrosive medium can be significantly increased in the charge transfer resistance on surface, in addition, surface microstructure shows excellent machinery surely
Qualitative, it is light that this will provide more stable wear-resisting property and corrosion resistance for super hydrophobic surface in actual use environment
Application of the metal material in marine corrosion and protection field provides important support.
Detailed description of the invention
Fig. 1 is the static contact angle for 5083 aluminum alloy surface of super-hydrophobic processing that the embodiment of the present invention mentions.
Fig. 2 is the energy Qwest figure of 5083 aluminium alloy of super-hydrophobic processing and blank sample that the embodiment of the present invention mentions；Wherein,
Scheme the energy Qwest that a is super-hydrophobic sample to scheme, figure b is that the energy Qwest of blank sample schemes.
Fig. 3 is the static contact angle for 5083 aluminum alloy surfaces that the embodiment of the present invention mentions.
Fig. 4 is the effect of mechanical stability figure for 5083 aluminum alloy surface of super-hydrophobic processing that the embodiment of the present invention mentions.
Specific embodiment
Below in conjunction with embodiment, the invention will be further described: what present embodiment was recorded is a kind of erosion resistant
The preparation method of super hydrophobic surface, the specific steps are as follows:
(1) pre-treatment is carried out to substrate surface: sample is placed in dehydrated alcohol and deionized water is cleaned by ultrasonic first, with
Afterwards using the SiC sand paper polishing matrix of different meshes (200,400,800,1200,2000)；
(2) oxalic acid aqueous solution constant pressure anodic oxidation: oxalic acid is dissolved in deionized water, 0.2-0.4mol/L electricity is prepared
Sample is then placed in bipolar electrode anodic oxidation system by electrolyte solution, and wherein sample is anode, and platinum electrode is cathode, reaction
System carries out anodic oxidation under 35-50V constant pressure, takes out sample after aoxidizing 5-15min, with deionized water and dehydrated alcohol point
Repeatedly remaining electrolyte solution Qing Xi not be removed；
(3) low-surface-energy molecular modification: compound concentration is the ethanol solution of the perfluoro decyl triethoxysilane of 1-3%,
Test piece is placed in the solution after impregnating 5-120min and is taken out；
(4) it is heat-treated: sample being placed in crucible in 100-200 DEG C of baking oven and is heated, taken after heating 10-60min
It is cooled to room temperature out, can be obtained the erosion resistant super hydrophobic surface.
Embodiment 1:
(1) to 5083 aluminum alloy surfaces carry out pre-treatment: first by 5083 aluminum alloy specimens be placed in dehydrated alcohol and go from
It is cleaned by ultrasonic in sub- water, then successively using the SiC sand paper polishing matrix of 200,400,800,1200,2000 different meshes；
(2) oxalic acid oxalic acid aqueous solution constant pressure anodic oxidation: is dissolved in the electrolysis that 0.3mol/L is prepared in deionized water
Sample is then placed in bipolar electrode anodic oxidation system by matter solution, wherein 5083 aluminium alloys are anode, platinum electrode is cathode,
Reaction system carries out anodic oxidation under 40V constant-pressure conditions, takes out sample after reacting 10min, with deionized water and anhydrous second
Alcohol is respectively washed repeatedly, removes remaining electrolyte solution；
(3) low-surface-energy molecular modification: the ethanol solution for the perfluoro decyl triethoxysilane that compound concentration is 1%, it will
Test piece is placed in the solution and takes out after immersion 20min；
(4) it is heat-treated: sample being placed in crucible in 120 DEG C of baking ovens and is heated, taken out after 20min and be cooled to room
Temperature can be obtained the erosion resistant aluminium base super hydrophobic surface.
The super hydrophobic surface being prepared is detected through contact angle measurement sessile drop method, static contact angle reaches 164.7 °
(as shown in Figure 1), and the static contact angle of untreated 5083 aluminium alloy is only 81.2 ° (as shown in Figure 3).
Application examples 1
Electrochemistry resistance is carried out to the super hydrophobic surface that above-mentioned substrate surface is formed using electrochemical workstation three-electrode system
The test of anti-spectrum, while the substrate not deal with (5083 aluminum alloy surface) is as compareing；
The three-electrode system, wherein embodiment 1 handles rear substrate or the substrate not dealt with is working electrode, platinum electricity
Extremely to electrode, saturated calomel electrode is reference electrode, and test frequency range is 105~10-2Hz (referring to fig. 2).
By the energy Qwest of super-hydrophobic 5083 aluminium alloy of Fig. 2 and blank sample figure as it can be seen that the capacitive reactance arc half of super hydrophobic surface
Diameter is significantly increased, and can obtain charge transfer resistance by the 3.56 × 10 of blank through data fitting4Ω·cm2It is promoted to 2.39 × 107
Ω·cm2, 3 orders of magnitude are increased, inhibition efficiency reaches 99.85%.
Application examples 2
The test that rear substrate carries out mechanical stability is handled to above-described embodiment 1:
Specifically: super-hydrophobic 5083 aluminium alloy being prepared is evaluated by the wear process under certain pressure load
Mechanical stability obtains substrate in above-described embodiment 1 and is placed on the sand paper of 1000 mesh, and load-bearing 100g physics carries above substrate
Substrate is moved 10cm along horizontal direction by promotion tool by lotus, then along the mobile 10cm of reversed horizontal direction, one
The abrasion distance of friction back and forth is 20cm, an as abrasion cycles, by between test surfaces contact angle and abrasion distance
Relationship (referring to fig. 4).
As shown in figure 4, the super hydrophobic surface being prepared as the result is shown is excellent in wear test under conditions, sample
150 ° or more are still maintained in the static contact angle Jing Guo 22 abrasion cycles rear surfaces, shows good mechanical stability.
Claims (7)
1. a kind of preparation method of erosion resistant super hydrophobic surface, which is characterized in that by the substrate after surface treatment with oxalic acid water
Solution as constant pressure anodic oxidation is carried out in electrolyte solution, low-surface-energy molecular modification is carried out after oxidation, heat treatment can be
Substrate surface forms erosion resistant super hydrophobic surface.
2. the preparation method of erosion resistant super hydrophobic surface according to claim 1, which is characterized in that the constant pressure anodic oxidation
It is placed in bipolar electrode anodic oxidation system for rear substrate will be surface-treated, using oxalic acid aqueous solution as electrolyte solution, substrate is
Anode, platinum electrode are cathode, 35-50V voltage anodic oxygen 5-15min.
3. the preparation method of erosion resistant super hydrophobic surface as described in claim 1 or 2, which is characterized in that the anodic oxidation
Afterwards by sample substrate, cleaned repeatedly respectively with deionized water and dehydrated alcohol.
4. the preparation method of erosion resistant super hydrophobic surface as described in claim 1 or 2, which is characterized in that the oxalic acid is water-soluble
Liquid concentration is 0.2-0.4mol/L.
5. the preparation method of erosion resistant super hydrophobic surface according to claim 1, which is characterized in that rear substrate room temperature will be aoxidized
Under be immersed in 5-120min in the ethanol solution of perfluoro decyl triethoxysilane, then take out at 100-200 DEG C at heating
Manage 10-60min.
6. by the preparation method of erosion resistant super hydrophobic surface described in claim 1 or 5, which is characterized in that the perfluoro decyl
Perfluoro decyl triethoxysilane concentration is 1-3% in the ethanol solution of triethoxysilane.
7. a kind of erosion resistant super-hydrophobic film of claim 1 the method preparation, it is characterised in that: according to described in claim 1
Method forms erosion resistant super-hydrophobic film in substrate surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910060768.0A CN109628978A (en) | 2019-01-22 | 2019-01-22 | A kind of preparation method of erosion resistant super hydrophobic surface |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910060768.0A CN109628978A (en) | 2019-01-22 | 2019-01-22 | A kind of preparation method of erosion resistant super hydrophobic surface |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109628978A true CN109628978A (en) | 2019-04-16 |
Family
ID=66063191
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910060768.0A Pending CN109628978A (en) | 2019-01-22 | 2019-01-22 | A kind of preparation method of erosion resistant super hydrophobic surface |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109628978A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113403661A (en) * | 2021-06-17 | 2021-09-17 | 中国计量大学 | Preparation method and application of titanium alloy anodic oxidation super-hydrophobic coating |
| CN115029767A (en) * | 2022-05-31 | 2022-09-09 | 珠海市湖大科技有限公司 | Preparation method of inorganic super-hydrophobic surface of aluminum alloy |
| CN116837382A (en) * | 2023-07-25 | 2023-10-03 | 中国船舶集团有限公司第七一九研究所 | Eutectic high-entropy alloy with wear-resistant superhydrophobic surface and preparation method thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101248219A (en) * | 2005-08-26 | 2008-08-20 | 财团法人神奈川科学技术研究院 | Porous polymer membrane, method for producing same, and method for manufacturing stamper used for production of same |
| CN101665968A (en) * | 2008-09-04 | 2010-03-10 | 中国科学院兰州化学物理研究所 | Process method for preparing ultra-hydrophobic surface by electrochemical method |
| CN102041509A (en) * | 2011-01-13 | 2011-05-04 | 中南大学 | Preparation method for constructing super-hydrophobic structure on surface of aluminum alloy |
| CN103276429A (en) * | 2013-06-24 | 2013-09-04 | 哈尔滨工业大学 | Preparation method of aluminum or aluminum alloy super-hydrophobic surface |
| CN103665415A (en) * | 2012-09-25 | 2014-03-26 | 黑龙江鑫达企业集团有限公司 | Preparation method of superhydrophobic microporous polymer film material |
| US20140110263A1 (en) * | 2012-10-19 | 2014-04-24 | University Of Pittsburgh | Superhydrophobic Anodized Metals and Method of Making Same |
| CN103818069A (en) * | 2012-11-16 | 2014-05-28 | 无锡市顺业科技有限公司 | Preparation method for super-hydrophobic coating |
| CN104726919A (en) * | 2013-12-20 | 2015-06-24 | 中国科学院兰州化学物理研究所 | Bionic micro-nano structure super hydrophobic aluminium surface preparation method |
| CN107964675A (en) * | 2016-10-20 | 2018-04-27 | 苏州汉力新材料有限公司 | The preparation method of super-hydrophobic anodised aluminium |
| CN109023472A (en) * | 2018-08-22 | 2018-12-18 | 中国科学院海洋研究所 | A kind of aluminium base method for preparing super-hydrophobic surface for characteristic of bouncing certainly with condensing droplet |
| CN109112599A (en) * | 2018-08-22 | 2019-01-01 | 大连理工大学 | A kind of preparation method obtaining sliding porous surface on aluminum substrate |
-
2019
- 2019-01-22 CN CN201910060768.0A patent/CN109628978A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101248219A (en) * | 2005-08-26 | 2008-08-20 | 财团法人神奈川科学技术研究院 | Porous polymer membrane, method for producing same, and method for manufacturing stamper used for production of same |
| CN101665968A (en) * | 2008-09-04 | 2010-03-10 | 中国科学院兰州化学物理研究所 | Process method for preparing ultra-hydrophobic surface by electrochemical method |
| CN102041509A (en) * | 2011-01-13 | 2011-05-04 | 中南大学 | Preparation method for constructing super-hydrophobic structure on surface of aluminum alloy |
| CN103665415A (en) * | 2012-09-25 | 2014-03-26 | 黑龙江鑫达企业集团有限公司 | Preparation method of superhydrophobic microporous polymer film material |
| US20140110263A1 (en) * | 2012-10-19 | 2014-04-24 | University Of Pittsburgh | Superhydrophobic Anodized Metals and Method of Making Same |
| CN103818069A (en) * | 2012-11-16 | 2014-05-28 | 无锡市顺业科技有限公司 | Preparation method for super-hydrophobic coating |
| CN103276429A (en) * | 2013-06-24 | 2013-09-04 | 哈尔滨工业大学 | Preparation method of aluminum or aluminum alloy super-hydrophobic surface |
| CN104726919A (en) * | 2013-12-20 | 2015-06-24 | 中国科学院兰州化学物理研究所 | Bionic micro-nano structure super hydrophobic aluminium surface preparation method |
| CN107964675A (en) * | 2016-10-20 | 2018-04-27 | 苏州汉力新材料有限公司 | The preparation method of super-hydrophobic anodised aluminium |
| CN109023472A (en) * | 2018-08-22 | 2018-12-18 | 中国科学院海洋研究所 | A kind of aluminium base method for preparing super-hydrophobic surface for characteristic of bouncing certainly with condensing droplet |
| CN109112599A (en) * | 2018-08-22 | 2019-01-01 | 大连理工大学 | A kind of preparation method obtaining sliding porous surface on aluminum substrate |
Non-Patent Citations (1)
| Title |
|---|
| YING WANG等: "Tribological Behaviors of Lubricants Modified Nanoporous Anodic Alumina Film", 《TRIBOL LETT》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113403661A (en) * | 2021-06-17 | 2021-09-17 | 中国计量大学 | Preparation method and application of titanium alloy anodic oxidation super-hydrophobic coating |
| CN115029767A (en) * | 2022-05-31 | 2022-09-09 | 珠海市湖大科技有限公司 | Preparation method of inorganic super-hydrophobic surface of aluminum alloy |
| CN115029767B (en) * | 2022-05-31 | 2023-12-29 | 湖北大学 | Preparation method of inorganic superhydrophobic surface of aluminum alloy |
| CN116837382A (en) * | 2023-07-25 | 2023-10-03 | 中国船舶集团有限公司第七一九研究所 | Eutectic high-entropy alloy with wear-resistant superhydrophobic surface and preparation method thereof |
| CN116837382B (en) * | 2023-07-25 | 2023-12-08 | 中国船舶集团有限公司第七一九研究所 | Eutectic high-entropy alloy with wear-resistant superhydrophobic surface and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Liu et al. | A novel combination approach for the preparation of superhydrophobic surface on copper and the consequent corrosion resistance | |
| CN103215614B (en) | Preparation method of metallic oxide anode containing cold spraying tantalum intermediate layer | |
| CN109628978A (en) | A kind of preparation method of erosion resistant super hydrophobic surface | |
| CN103952732B (en) | Metal super-hydrophobic surface and preparation method thereof | |
| CN100564609C (en) | The method of silane reinforcing magnesium alloy cathode electrophoretic corrosion-proof layer | |
| CN101429672A (en) | Surface treating method for sea water corrosion-resistant metal aluminum or aluminum alloy | |
| CN104131322A (en) | Aluminum product surface super-hydrophobic film and making method thereof | |
| CN102817063A (en) | Preparation method for light green superhydrophobic corrosion-resistant film on surface of magnesium-lithium alloy | |
| CN103305786A (en) | Low-temperature and low-pressure ion nitriding method and device for stainless steel workpiece | |
| Pak et al. | Effect of organic additives on structure and corrosion resistance of MAO coating | |
| CN102304741A (en) | Anodic oxidation method for preparing aluminum-based super-hydrophobic film | |
| CN112553664B (en) | Aluminum alloy part with layered double hydroxide-graphene oxide silane composite coating and preparation method thereof | |
| CN105331941A (en) | Micro-arc oxidation method for surfaces of copper, copper alloy, zinc and zinc alloy | |
| CN104264196A (en) | Method for preparing super-hydrophobic membrane layer on surface of magnesium alloy through one-step method as well as alloy and application of uper-hydrophobic membrane layer | |
| CN107855254A (en) | A kind of preparation method of the corrosion-resistant organic composite coating of Mg alloy surface | |
| CN106086996A (en) | A kind of reparation has been got rusty the composite surface treatment method of passivation for stainless steel state | |
| CN107937903A (en) | A kind of preparation method of corrosive protection of aluminium alloy layer | |
| CN107955960A (en) | A kind of preparation method of aluminum alloy surface multiple-protection layer | |
| CN103938254A (en) | Preparation method of connecting corrosion-resisting micro-arc oxidation layer on surface of magnesium alloy | |
| CN107142467A (en) | A kind of preparation method of super lubrication aluminium surface | |
| CN105316741B (en) | A kind of method for carrying out surface by micro-arc oxidation processing to aluminium alloy using grading current | |
| CN109338451A (en) | A kind of aluminium base is anticorrosive, antimicrobial attachment super-hydrophobic film and preparation method thereof | |
| CN108707933A (en) | The galvanizing flux and preparation method thereof of super-hydrophobic zinc-plated carbon steel | |
| CN103147112A (en) | Electrolyte as well as application and method for preparing micro-arc oxidation film on zirconium alloy cladding of nuclear fuel rod by an electrolyte | |
| CN111020664B (en) | Preparation method of graphene-containing micro-arc oxidation corrosion-resistant ceramic layer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190416 |