CN106399986A - Preparation method of super-hydrophobic aluminum surface with self-cleaning function - Google Patents
Preparation method of super-hydrophobic aluminum surface with self-cleaning function Download PDFInfo
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- CN106399986A CN106399986A CN201611094508.8A CN201611094508A CN106399986A CN 106399986 A CN106399986 A CN 106399986A CN 201611094508 A CN201611094508 A CN 201611094508A CN 106399986 A CN106399986 A CN 106399986A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/02—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using non-aqueous solutions
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/78—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/20—Acidic compositions for etching aluminium or alloys thereof
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
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- ing And Chemical Polishing (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention belongs to the technical field of surface treatment, and relates to a preparation method of a super-hydrophobic aluminum surface with a self-cleaning function. The preparation method comprises the following steps: (1) pretreatment: grinding, cleaning and drying an aluminum sample in sequence to obtain a clean sample; (2) chemical etching: putting the sample subjected to pretreatment into a chloridized molten iron solution for soaking at room temperature, then taking out the sample to clear away dirt on the surface, and drying the sample in air; and (3) surface modification: placing the sample subjected to chemical etching treatment into a low-surface-energy reagent for soaking at the room temperature for 1 to 2 h to form a layer of hydrophobic thin film on the surface of the sample, then taking out the sample, and placing the sample into a constant-temperature drying box for drying to obtain the super-hydrophobic surface. The preparation process is simple, and the raw materials are readily available; preparation of the super-hydrophobic aluminum surface with the self-cleaning function can be realized under an atmospheric environment; the contact angle for water is about 150 degrees; and the prepared super-hydrophobic aluminum surface with the self-cleaning function is good in self-cleaning and hydrophobization effect.
Description
Technical field
The invention belongs to technical field of surface, more particularly, to a kind of Super-hydrophobic aluminium surface with self-cleaning function
Preparation method.
Background technology
The eighties in 20th century, botanist Barthlott and Neihuis of Univ Bonn Germany is by tying to lotus leaf surface
The observation of structure finds the raised and wax-like organizational structure of micron order that its surface exists so that Folium Nelumbinis have super-hydrophobicity (i.e. water
It is dropped in leaf surfaces and can automatically be gathered into the globule and be rolled down) cause worldwide very big concern.It has been investigated that
Super-hydrophobic phenomenon in nature is seen everywhere, the leaf of Oryza sativa L., sharkskin, the wing of butterfly, the leg of water skipper, cicada's wings surface
All there is superhydrophobic microstructure surface.These micro-structure surfaces have special property, such as self-cleaning property, non-stick nature, subtract
Resistive etc..If the good characteristic of super hydrophobic surface is applied to the serviceability that engineering is greatly improved material in practice, such as
Super hydrophobic surface is used for skyscraper glass, the automatically cleaning effect of achievable rain drop erosion, reduces the loss of manpower and materials.
Aluminum and its alloy are a kind of very important engineering metal materials, with its light weight, specific strength is high, the thermal efficiency is good,
Easy processing molding, the excellent performance of corrosion resistance are widely used in various fields.There is the aluminum of super hydrophobic surface and aluminum closes
Gold has excellent self-cleaning performance and decay resistance, can be widely applied to automobile, ship, building, Aero-Space and machinery
The industrial circles such as manufacture.The preparation of Super-hydrophobic aluminium sill at present mainly adopts surface-coating technology so that hydrophobic performance is inadequate
Ideal also has the problem of matrix and the adhesion applying interlayer simultaneously.Therefore remain a need for development low cost and preparation process is simple
Super-hydrophobic aluminium surface preparation method.
The preparation method of metal current substrate superhydrophobic surface mainly have chemical etching method, anodizing, vapour deposition process,
Laser ablation method etc..Chemistry etch techniques are because of its preparation process is simple, reproducible, low cost, wide adaptability and be subject to people
Extensive concern.Patent as Application No. 201010521109.1 discloses at a kind of superhydrophobic surface of aluminum alloy of low cost
Reason method, carries out chemical etching using aqueous hydrochloric acid solution to aluminum alloy surface, utilizes long-chain fatty acid pair by vapour deposition method afterwards
Sample surfaces carry out being deposited with modification and being obtained have well hydrophobic aluminum alloy surface.Application No. 201610073380.0 special
Profit discloses a kind of preparation method of the aluminum surface super hydrophobic coating with micro-nano compound structure, and the method is first to immerse aluminium flake
Etch in acid etch liquid, then be immersed in nano-particle solution, multiple to having micro-nano through high-temperature process and silylation modification
Close the Super-hydrophobic aluminium surface of structure.The patent of Application No. 201210031621.7 discloses a kind of metallic aluminium bionic super-hydrophobic table
Noodle producing method, the method profit the method is that the aluminium flake cleaning up is placed in certain density hydrochloric acid or sodium hydroxide solution
Soak to remove the oxide layer of material surface, be then hung up chemical etching one night in cerous nitrate and pregnancy urotropine mixed solution,
The super hydrophobic surface that contact angle is 150 ° 165 ° is obtained after Stearate Modified.The patent of Application No. 201410667574.4
Disclose a kind of construction high stable Super-hydrophobic aluminium surface method, the method is first aluminium flake to be put in sodium hydroxide solution alkaline etching again
As for acid etching in salpeter solution, then immersed again in ammonia in aluminum flake surface deposited oxide aluminium film by anodised method
Chemical attack, by silicon fluoride modify to super hydrophobic surface.
The preparation method of above-described super hydrophobic surface all can obtain preferably super-hydrophobic effect, but there is also some and ask
Topic.Example hydrochloric acid belongs to hazardous chemical articles for use, contacts its steam or smog can cause the feelings such as acute poisoning, epistaxiss, gingiva bleeding gingival hemorrhage
Condition, wrongly takes and digestive tract can be caused to burn, and situations such as gastric perforation, needs careful during use.Preparing super hydrophobic surface using coating needs
Consider matrix material and the problem applying inter-layer bonding force, be also easy to produce peeling when coating is acted on external force.Application No.
201210031621.7 and 201410667574.4 patent complex technical process, processing cost is big, is unfavorable for large-scale production.
Therefore, how to prepare stable super-hydrophobic automatic cleaning surface using simple method, meet its answering in industrial aspect
With being particularly important.
Content of the invention
For solving the defect of the Super-hydrophobic aluminium surface preparation technology complexity that prior art exists, the present invention provides one kind to have
The preparation method on the Super-hydrophobic aluminium surface of self-cleaning function.
For solving above-mentioned technical problem, the technical solution adopted in the present invention is：A kind of have the super thin of self-cleaning function
The preparation method of water aluminium surface, step is as follows：
(1) pretreatment：Aluminum sample is obtained successively after polishing, clean, being dried the sample of cleaning；
(2) chemical etching：Sample after pretreatment is put in ferric chloride in aqueous solution, soaks at room temperature, further take out
Remove surface contaminants, and air-dry；
(3) surface modification：Sample after chemical etching is processed be placed in low-surface-energy reagent soak 1 at room temperature～
2h, makes sample surfaces form one layer of hydrophobic film, then takes out and puts into dry in constant temperature oven, i.e. prepared Super-hydrophobic aluminium surface.
Specifically, the pre-treatment step described in step (1) is specially aluminum sample successively through 400#、1000#、3000#Sand paper
Polishing, the sample after grinding process carries out ultrasound wave with dehydrated alcohol and distilled water successively again and cleans, and ultrasonic temperature is 40～
60 DEG C, the time is 15～30min, then 20～30min is dried in 50～80 DEG C of constant temperature ovens, obtains the sample of cleaning.
Preferably, the concentration of the ferric chloride in aqueous solution described in step (2) is 1.4～1.5mol/L, sample is in iron chloride
30-60min is soaked in aqueous solution.
Further, the removing surface contaminants described in step (2) concretely comprise the following steps, and will soak the sample after ferric chloride in aqueous solution
Product take out to put in ultrasonic cleaning agent and are cleaned by ultrasonic 5-10min under 40-60 DEG C of constant temperature with dehydrated alcohol, distilled water successively.
Preferably, the low-surface-energy reagent described in step (3) is 1H, 1H, 2H, 2H- perfluoro decyl triethoxysilane
Ethanol solution, stearic ethanol solution, the ethanol solution of cetyl trimethyl silane, 17 fluorine decyl trimethoxy silicon
One of ethanol solution of the ethanol solution of alkane, lauric ethanol solution and Palmic acid.
Preferably, the mass percent of the low-surface energy substance in described low-surface-energy reagent is 1%-2%.
Preferably, the drying described in step (3) is adjusted to 20-30min be dried in 130 DEG C of constant temperature oven.
Specifically, step (2) and the room temperature described in step (3) are 60%-80% for air humidity, and ambient temperature is 20-
26℃.
Beneficial effect：Preparation process is simple, raw material are easy to get.The side being combined using chemistry etch techniques and surface modification
Method, can achieve the preparation on the Super-hydrophobic aluminium surface with self-cleaning function under atmospheric environment；Obtained has automatically cleaning
The Super-hydrophobic aluminium surface of function has coarse micro structure, is 150 ° about to the contact angle of water；Obtained has automatically cleaning
There are excellent automatically cleaning and hydrophobic effect in the Super-hydrophobic aluminium surface of function, water be dropped in sample surfaces will not stagnate motionless, but
Tumble rapidly and take away dust and the dirt on surface, the time of contact of alloy matrix aluminum and water droplet can be reduced simultaneously, reduce rotten
Lose, increase its serviceability.
Brief description
Fig. 1 is the micro-structure diagram on the Super-hydrophobic aluminium surface of example 1 gained；
Fig. 2 is the contact angle schematic diagram on the Super-hydrophobic aluminium surface of example 1 gained；
Fig. 3 is that iron chloride etches sample, copper chloride etches the comparison diagram of sample and not etched sample；
Fig. 4 is the comparison diagram of the self-cleaning that iron chloride etches sample, copper chloride etching sample and not etched sample.
Specific embodiment
In order to be better understood from the present invention, below in conjunction with example, technical scheme is done with further details of Jie
Continue.Described in following embodiments, experimental technique is conventional method if no special instructions, described reagent and material such as no special theory
Bright all can obtain from commercial channels.
Embodiment 1
A kind of preparation method on Super-hydrophobic aluminium surface with self-cleaning function of the present embodiment, comprises the steps：
(1) pretreatment：By 6061 aluminum alloy sheets successively through 400#、1000#、3000#Sand papering, after grinding process
Sample carries out ultrasound wave with dehydrated alcohol and distilled water successively and cleans, and ultrasonic temperature is 50 DEG C, and the time is 20min, then at 80 DEG C
10min is dried in constant temperature oven, obtains the sample of cleaning；
(2) chemical etching：Described clean sample is put in 1.4mol/L ferric chloride in aqueous solution, soaks under room temperature environment
Bubble 60min.Taking-up put in ultrasonic washing unit successively with dehydrated alcohol, distilled water be cleaned by ultrasonic under 60 DEG C of constant temperature 5min with
Remove surface contaminants, and air-dry；
(3) surface modification：Sample after chemical treatment is placed in 2% 1H, 1H, 2H, 2H- perfluoro decyl triethoxysilicane
Soak 1h at room temperature in alkane ethanol solution, make sample surfaces form one layer of hydrophobic film, then take out and put into 130 DEG C about
30min is dried in constant temperature oven, that is, the described Super-hydrophobic aluminium surface with self-cleaning function is obtained.
The micro-structure diagram on the Super-hydrophobic aluminium surface with self-cleaning function that this example is obtained is as shown in figure 1, surface is in
Micron order coarse structure.
The contact angle on the Super-hydrophobic aluminium surface with self-cleaning function that this example is obtained is as shown in Fig. 2 contact with water
Angle is 149 °.
Comparative example 1
In order to be contrasted with embodiment 1, the ferric chloride in aqueous solution of the chemical etching liquid 1.4mol/L in embodiment 1 is replaced
It is changed to the copper chloride solution of 1.4mol/L, and the etching reaction time is replaced with 30s and (finds that copper chloride solution is carved through test
The optimum reacting time of erosion aluminum alloy sample is 30s, reacts insufficient less than 30s, higher than 30s overresponse, all affects it and connect
Feeler value), other conditions are with embodiment 1.
By comparing discovery：
1., when being used copper chloride to be reacted as etching liquid, its reaction is relatively more violent, the more difficult control of reaction rate；And
Iron chloride reacts its reaction rate more gentle, easily controllable.
2. the contact angle of the sample of copper chloride etching is 146 °, and the contact angle of the sample of iron chloride etching is 149 °, because
The hydrophobicity of this sample using iron chloride etching is better than copper chloride.
3. Fig. 3 be from left to right followed successively by iron chloride etching aluminum alloy sample, copper chloride etching aluminum alloy sample, without
The aluminum alloy sample figure of etching.For comparing the self-cleaning size of two methods, at room temperature, three sample surfaces are all spread one
Layer sandy soil, then drip about 10 μ l about pure water, and angle certain for sample inclination is observed their automatically cleaning situation.Fig. 4
Etch the comparison diagram of the self-cleaning of sample, copper chloride etching sample and not etched sample for iron chloride.Find in chlorine through comparing
Change the sample surfaces of ferrum etching, the sandy soil along road can be taken away when water droplet tumbles, self-cleaning is best.Sample table in copper chloride etching
Face, can take away most of dust when water droplet tumbles, still have fraction dust to keep sample surfaces.Not modified sample surfaces
Self-cleaning is poor, and dust and water mix, and remain in sample surfaces.
4. the commercially available price of copper chloride is 4 times of iron chloride price, and comparatively speaking the cost performance of iron chloride is higher.
Embodiment 2
(1) pretreatment：By 6061 aluminum alloy sheets successively through 400#、1000#、3000#Sand papering, after grinding process
Sample carries out ultrasound wave with dehydrated alcohol and distilled water successively and cleans, and ultrasonic temperature is 40 DEG C, and the time is 30min, then at 50 DEG C
20min is dried in constant temperature oven, obtains the sample of cleaning；
(2) chemical etching：Described clean sample is put in 1.5mol/L ferric chloride in aqueous solution, soaks under room temperature environment
Bubble 30min.Taking-up is put in ultrasonic washing unit and is cleaned by ultrasonic 10min under 40 DEG C of constant temperature with dehydrated alcohol, distilled water successively
To remove surface contaminants, and air-dry；
(3) surface modification：Ethanol sample after chemical treatment being placed in 1% 17 fluorine decyl trimethoxy silanes is molten
Soak 2h at room temperature in liquid, make sample surfaces form one layer of hydrophobic film, then take out the constant temperature oven putting into 130 DEG C about
In 20min is dried, that is, the described Super-hydrophobic aluminium surface with self-cleaning function is obtained.The sample being finally obtained after tested and water
Contact angle be 148 °.
Claims (8)
1. a kind of preparation method on the Super-hydrophobic aluminium surface with self-cleaning function it is characterised in that：Step is as follows：
(1) pretreatment：Aluminum sample is obtained successively after polishing, clean, being dried the sample of cleaning；
(2) chemical etching：Sample after pretreatment is put in ferric chloride in aqueous solution, soaks at room temperature, further take out removing
Surface contaminants, and air-dry；
(3) surface modification：Sample after chemical etching is processed is placed in low-surface-energy reagent and soaks 1～2h at room temperature, makes
Sample surfaces form one layer of hydrophobic film, then take out and put into dry in constant temperature oven, i.e. prepared Super-hydrophobic aluminium surface.
2. the Super-hydrophobic aluminium surface with self-cleaning function according to claim 1 preparation method it is characterised in that：Step
Suddenly the pre-treatment step described in (1) is specially aluminum sample successively through 400#、1000#、3000#Sand papering, after grinding process
Sample carry out ultrasound wave with dehydrated alcohol and distilled water successively again and clean, ultrasonic temperature is 40～60 DEG C, the time is 15～
30min, then 20～30min is dried in 50～80 DEG C of constant temperature ovens, obtain the sample of cleaning.
3. the Super-hydrophobic aluminium surface with self-cleaning function according to claim 1 preparation method it is characterised in that：Step
Suddenly the concentration of the ferric chloride in aqueous solution described in (2) is 1.4～1.5mol/L, and sample soaks 30- in ferric chloride in aqueous solution
60min.
4. the preparation method on the Super-hydrophobic aluminium surface with self-cleaning function according to claim 1 or 3, its feature exists
In：Removing surface contaminants described in step (2) concretely comprise the following steps, and the sample taking-up after immersion ferric chloride in aqueous solution are put into ultrasonic
It is cleaned by ultrasonic 5-10min with dehydrated alcohol, distilled water under 40-60 DEG C of constant temperature successively in ripple abluent.
5. the Super-hydrophobic aluminium surface with self-cleaning function according to claim 1 preparation method it is characterised in that：Step
Suddenly the low-surface-energy reagent described in (3) is 1H, the ethanol solution of 1H, 2H, 2H- perfluoro decyl triethoxysilane, stearic
Ethanol solution, the ethanol solution of cetyl trimethyl silane, the ethanol solution of 17 fluorine decyl trimethoxy silanes, lauric acid
Ethanol solution and Palmic acid one of ethanol solution.
6. there is the preparation method on the Super-hydrophobic aluminium surface of self-cleaning function according to claim 1 or 5, its feature exists
In：The mass percent of the low-surface energy substance in described low-surface-energy reagent is 1%-2%.
7. the Super-hydrophobic aluminium surface with self-cleaning function according to claim 1 preparation method it is characterised in that：Step
Suddenly the drying described in (3) is adjusted to 20-30min be dried in 130 DEG C of constant temperature oven.
8. the Super-hydrophobic aluminium surface with self-cleaning function according to claim 1 preparation method it is characterised in that：Step
Suddenly (2) and the room temperature described in step (3) are 60%-80% for air humidity, and ambient temperature is 20-26 DEG C.
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| CN107649352A (en) * | 2017-09-19 | 2018-02-02 | 重庆大学 | A kind of fast method for preparing of the super-hydrophobic extreme wetability aluminum alloy materials of large scale |
| CN107899921A (en) * | 2017-11-07 | 2018-04-13 | 江苏理工学院 | A kind of preparation method on the Super-hydrophobic aluminium surface with deicing properties |
| CN109456738A (en) * | 2018-12-18 | 2019-03-12 | 长安大学 | A kind of preparation method and aluminium base suppression frost experimental system of super-hydrophobic aluminium base |
| CN109468648A (en) * | 2018-12-29 | 2019-03-15 | 哈尔滨工业大学 | The large-scale producing method on aluminum or aluminum alloy antifrost surface |
| CN109518175A (en) * | 2018-11-29 | 2019-03-26 | 鲁东大学 | A kind of super-hydrophobic coating for metal surfaces and preparation method thereof |
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