CN106987875A - A kind of preparation method of super-hydrophobic superoleophobic material - Google Patents
A kind of preparation method of super-hydrophobic superoleophobic material Download PDFInfo
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- CN106987875A CN106987875A CN201710123834.5A CN201710123834A CN106987875A CN 106987875 A CN106987875 A CN 106987875A CN 201710123834 A CN201710123834 A CN 201710123834A CN 106987875 A CN106987875 A CN 106987875A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
Abstract
The present invention relates to a kind of technical field of new material preparation, specially a kind of preparation method of super-hydrophobic superoleophobic material.Methods described step is as follows：Make anode and negative electrode respectively with premenstrual treated copper sheet and sheet metal, using the aqueous solution containing nickel ion copper ion as electrolyte, electro-deposition is carried out at constant current, then cathodic metal sheet base is taken out to place into after cleaning, drying and a period of time is soaked in chain alkyl siloxanes ethanol solution, you can obtain the material with super-hydrophobic superoleophobic performance.Preparation technology used in the present invention is simple, time-consuming short, and the super-hydrophobic superoleophobic performance of material is stable, persistently, with higher economic value.
Description
Technical field
The present invention relates to a kind of technical field of new material preparation, specially a kind of preparation side of super-hydrophobic-superoleophobic material
Method.
Background technology
By " lotus leaf effect " in nature triggered people to super hydrophobic surface study, in research process it is found that
Super hydrophobic material surface has the characteristics such as automatically cleaning, freezing frosting, corrosion-resistant, drag reduction, high-bearing capacity, in military, communication, energy
The fields such as source, environment suffer from being widely applied prospect.But with going deep into for research, it has been found that common super hydrophobic surface is present
Some weakness, such as：Only there is the super-hydrophobic material without superoleophobic performance, it is easily oily when in face of there is the waste water of greasy dirt
Dirt is polluted and loses ultra-hydrophobicity, material is lost original premium properties quickly.Therefore, preparation only has super-hydrophobicity
The material of energy can not meet the demand of industrial development, prepare a kind of material with super-hydrophobic and superoleophobic dual property
As a kind of research tendency.
The content of the invention
The goal of the invention of the present invention is that there is provided a kind of preparation method of super-hydrophobic-superoleophobic material for problem above.
The present invention concrete technical scheme be：
A kind of preparation method of super-hydrophobic-superoleophobic material, this method comprises the following steps：Super-hydrophobic-superoleophobic material with
Metal is substrate, and the micro-nano coarse structure coating of sheet metal is assigned using electrodeposition process, then to put it into silicon fluoride-ethanol molten
Immersion modification a period of time in liquid, take out drying and obtain the material with super-hydrophobic-superoleophobic performance.
A kind of preparation method of super-hydrophobic-superoleophobic material, this method specifically includes following steps：
A, substrate pretreatment
Size identical copper sheet and metal sheet substrate are cleaned by ultrasonic in acetone, ethanol and deionized water respectively, surface is removed
Greasy dirt；Then sheet metal is polished with the mesh sand paper mechanical grinding physics of 300 mesh ~ 1200, places into chemistry in acid or aqueous slkali and throw
Light, deionized water rinsing is clean, dries up standby；
B, electrolyte quota
In deionized water, a certain amount of nickel salt is sequentially added while stirring, mantoquita, sodium hypophosphite, citric acid, surface is lived
Property agent and conductive materials, 5.0 ~ 6.0 are adjusted to alkaline solution by pH values；
C, prepare coating
Anode is made with copper sheet, sheet metal makees negative electrode, be put into electrolyte and electroplated；Current density control exists
0.03A/cm2~0.10A/cm2, electrodeposition time 3 ~ 30 minutes, cathode substrate is gone out by deposition growth special micro-nano
The coating of rice coarse structure；
D, modification coating
Obtained coating is immersed in 0.5h ~ 5h in 0.1wt% ~ 1.5wt% chain alkyl siloxanes ethanol solutions, taken out with 30 DEG C
~ 80 DEG C of constant temperature oven drying obtain super-hydrophobic-superoleophobic material.
The preparation of the super-hydrophobic-superoleophobic material is divided into two steps, and it is special that the first step assigns matrix by electrochemical deposition method
The coating of micro-nano coarse structure；Matrix is put into silicon fluoride ethanol solution and modify obtaining super-double-hydrophobic surface material by second step
Material.
Described sheet metal is aluminium flake, iron plate, stainless steel substrates, zinc metal sheet or titanium sheet.
In described electrolyte configuration step, nickel salt is nickel sulfate or nickel halogenide；Mantoquita is copper sulphate or copper chloride；Surface
Activating agent is lauryl sodium sulfate or neopelex；Conductive materials are sodium sulphate or sodium chloride；Alkaline solution is
Ammoniacal liquor or sodium hydroxide.
Each chemical agent concentration is：Nickel salt：0.05 ~ 0.15M, mantoquita：0.05 ~ 0.15M, sodium hypophosphite：0.01~
0.05M, citric acid：0.01 ~ 0.10M, surfactant：0.5 ~ 0.15g/L, conductive materials：0.06~0.12M.
The chain alkyl silicone agent be dodecyltrimethoxysilane, hexadecyl trimethoxy silane and
Any one or a few mixture in octadecyl trimethoxysilane.
The positive effect of the present invention is embodied in：
（One）, preparation method it is simple, take short, experiment parameter is controllable, and the performance of material is stable, persistently.
（Two）, with wide market, available for field of Environment Protection many aspects.
Brief description of the drawings
Fig. 1 is the electron scanning micrograph of the super-hydrophobic-superoleophobic material surface prepared in embodiment 1.
Fig. 2 tests photo for super-hydrophobic-superoleophobic material surface water droplet and oil droplet prepared in embodiment 1.Left side
Drop is water, and right side drop is oil.
Embodiment
With reference to embodiment, the present invention is further described, but does not limit the scope of the invention.
Embodiment 1：
A, substrate pretreatment：Copper sheet, aluminium flake are cut into 5cm × 3.5cm × 0.1cm sizes, in acetone, ethanol and gone respectively
It is cleaned by ultrasonic 15min in ionized water, removes surface and oil contaminant.Then by sheet metal respectively with 300 mesh, 600 mesh and 1200 mesh sand paper
Sanding and polishing, places into chemical polishing 5min in 2mol/L sodium hydroxides, and deionized water rinsing is clean, dries up standby；
B, electrolyte quota：In 100ml deionizations, stirring sequentially adds 0.1M nickel sulfate hexahydrates, the water sulphur of 0.0625M five simultaneously
Sour copper, 0.10M sodium sulphate, 0.025M sodium hypophosphites, 0.05M citric acids, 0.012g lauryl sodium sulfate agent, 25wt%
Solution ph will be adjusted to 5.5 by ammoniacal liquor.
C, prepare coating：Anode is made with copper sheet, sheet metal makees negative electrode, add electrolyte and electroplated；Current density control
System is in 0.06A/cm2, electrodeposition time 10min, cathode substrate goes out to have special micro and nano coarse structure by deposition growth
Coating.
D, modification coating：Obtained coating is immersed in 0.8wt% dodecyltrimethoxysilane ethanol solutions and reacted
3h, takes out and obtains super-hydrophobic-superoleophobic material in 60 DEG C of constant temperature oven drying.
Embodiment 2：
A, substrate pretreatment：Copper sheet, stainless steel substrates are cut into 5.2cm × 3.5cm × 0.1cm sizes, respectively in acetone, second
It is cleaned by ultrasonic 15min in alcohol and deionized water, removes surface and oil contaminant.Then by sheet metal respectively with 300 mesh, 600 mesh and 1200
Mesh sand paper sanding and polishing, places into chemical polishing 2min in 8mol/L hydrochloric acid, and deionized water rinsing is clean, dries up standby；
B, electrolyte quota：In 100ml deionizations, stir and sequentially add 0.15M nickel chlorides simultaneously, 0.05M copper chlorides,
0.06M sodium chloride, 0.05M sodium hypophosphites, 0.01M citric acids, 0.015g lauryl sodium sulfate, 0.1M sodium hydroxide are incited somebody to action
Solution ph is adjusted to 5.
C, prepare coating：Anode is made with copper sheet, sheet metal makees negative electrode, add electrolyte and electroplated；Current density control
System is in 0.03A/cm2, electrodeposition time 30min, cathode substrate goes out to have special micro and nano coarse structure by deposition growth
Coating.
D, modification coating：Obtained coating is immersed in 0.1wt% octadecyl trimethoxysilane ethanol solutions and reacted
5h, takes out and obtains super-hydrophobic-superoleophobic material in 60 DEG C of constant temperature oven drying.
Embodiment 3：
A, substrate pretreatment：Copper sheet, titanium are cut into 5.2cm × 3.5cm × 0.1cm sizes, in acetone, ethanol and gone respectively
It is cleaned by ultrasonic 15min in ionized water, removes surface and oil contaminant.Then by sheet metal respectively with 300 mesh, 600 mesh and 1200 mesh sand paper
Sanding and polishing, places into chemical polishing 5min in 2mol/L hydrofluoric acid, and deionized water rinsing is clean, dries up standby；
B, electrolyte quota：In 100ml deionizations, stirring sequentially adds 0.05M six hydration nickel sulfates, the water of 0.15M five simultaneously
Close copper sulphate, 0.12M sodium sulphate, 0.01M sodium hypophosphites, 0.1M citric acids, 0.005g neopelexes, 25%
Solution ph is adjusted to 6 by ammoniacal liquor.
C, prepare coating：Anode is made with copper sheet, sheet metal makees negative electrode, add electrolyte and electroplated；Current density control
System is in 0.1A/cm2, electrodeposition time 3min, cathode substrate goes out to have the plating of special micro and nano coarse structure by deposition growth
Layer.
D, modification coating：Obtained coating is immersed in 1.5wt% hexadecyl trimethoxy silanes and 0.1% octadecyl
0.5h is reacted in the ethanol solution of trimethoxy silane, takes out and obtains super-hydrophobic-superoleophobic material in 60 DEG C of constant temperature oven drying.
Embodiment 4：
It is identical with the condition of embodiment 1, but copper sulphate or the metal ion species of nickel sulfate one are only added in electrolyte, remaining step is complete
Unanimously.The result is that only plus sulfuric acid electrodeposition of nickel coating surface after tested water contact angle be 90.1 °, do not reach super-hydrophobic.Only
Plus water contact angle is 152.7 ° to the coating surface of copper sulphate electro-deposition after tested, although it is but not superoleophobic to show super-hydrophobic oil,
Main cause is when we only add a metal ion species and deposited, and only a kind of fixed structure is in growth, and we are simultaneously
Two kinds of deposition is even more more, and every kind of material formation speed or growth pattern are different to cause final surface texture different, is formed
Special coarse structure, so as to super-hydrophobic while superoleophobic.
Embodiment 5：
It is identical with the condition of embodiment 1, but change the nickel sulfate hexahydrate concentration in electrolyte into 0.01 M.Remaining step complete one
Cause.The result is that coating surface is not super-hydrophobic but superoleophobic after tested after electro-deposition.Its main cause is six water sulphur in electrolyte
The concentration of sour nickel is too low, and main or copper deposition can not grow the micro-nano coarse structure special into embodiment 1, therefore not
Can reach simultaneously it is super-hydrophobic-superoleophobic, only when we cupro-nickel ion ratio control could generate spy within limits
Different micro-nano coarse structure is so as to realize super-amphiphobic.
Embodiment 6：
It is identical with the condition of embodiment 1, but the aluminium flake after deposition is immersed in 0.1wt% octadecyl trimethoxysilane ethanol
10min is reacted in solution, remaining step is completely the same.The result is that coating surface water contact angle is about 120 ° after electro-deposition, oil
Drop can be attached on coating, it is impossible to reach super-hydrophobic-superoleophobic effect.Although main cause is cathode substrate, deposition growth goes out
The coating of special micro and nano coarse structure, when coating is immersed in, the reaction time in low-surface energy substance is too short, and the surface of coating does not have
Have abundant with the reaction of octadecyl trimethoxysilane ethanol solution, without sufficiently low surface energy.
Embodiment 7：
Identical with the condition of embodiment 1, but electrodeposition time 1h, remaining step is completely the same.The result is that coating table after electro-deposition
Face locally reaches super-hydrophobic-superoleophobic effect.Main cause is where appropriate, electricity when concentration of electrolyte proportioning with current density control
Sedimentation time is long, causes the micro-nano coarse structure originally formed to be capped, and it is heavy loosely organized fine particle occur
Product is on surface, it is easy to which the mechanical strength that drops is low, and surface topography is easy to be broken ring, and part surface can show super-hydrophobic-super
The effect of oleophobic.
Claims (6)
1. a kind of preparation method of super-hydrophobic-superoleophobic material, it is characterised in that methods described comprises the following steps：This is super thin
Water-superoleophobic material assigns the micro-nano coarse structure coating of sheet metal, then put using metal as substrate using electrodeposition process
Enter immersion modification a period of time in silicon fluoride-ethanol solution, take out drying and obtain the material with super-hydrophobic-superoleophobic performance；
Specifically include following steps：
A, substrate pretreatment
Size identical copper sheet and metal sheet substrate are cleaned by ultrasonic in acetone, ethanol and deionized water respectively, surface is removed
Greasy dirt；Then sheet metal is polished with the mesh sand paper mechanical grinding physics of 300 mesh ~ 1200, places into chemistry in acid or aqueous slkali and throw
Light, deionized water rinsing is clean, dries up standby；
B, electrolyte quota
In deionized water, a certain amount of nickel salt is sequentially added while stirring, mantoquita, sodium hypophosphite, citric acid, surface is lived
Property agent and conductive materials, 5.0 ~ 6.0 are adjusted to alkaline solution by pH values；
C, prepare coating
Anode is made with copper sheet, sheet metal makees negative electrode, be put into electrolyte and electroplated；Current density control exists
0.03A/cm2~0.10A/cm2, electrodeposition time 3 ~ 30 minutes, cathode substrate is gone out by deposition growth special micro-nano
The coating of rice coarse structure；
D, modification coating
Obtained coating is immersed in 0.5h ~ 5h in 0.1wt% ~ 1.5wt% chain alkyl siloxanes ethanol solutions, taken out with 30 DEG C
~ 80 DEG C of constant temperature oven drying obtain super-hydrophobic-superoleophobic material.
2. the preparation method of super-hydrophobic-superoleophobic material as claimed in claim 1, it is characterised in that：Super-hydrophobic-superoleophobic material
Preparation be divided into two steps, the first step passes through the coating that electrochemical deposition method assigns matrix special micro and nano coarse structure；Second step
Matrix is put into silicon fluoride ethanol solution and modify obtaining super-double-hydrophobic surface material.
3. the preparation method of super-hydrophobic-superoleophobic material as claimed in claim 1, it is characterised in that：Described sheet metal is
Aluminium flake, iron plate, stainless steel substrates, zinc metal sheet or titanium sheet.
4. the preparation method of super-hydrophobic-superoleophobic material as claimed in claim 1, it is characterised in that：Described electrolyte configuration
In step, nickel salt is nickel sulfate or nickel halogenide；Mantoquita is copper sulphate or copper chloride；Surfactant be lauryl sodium sulfate or
Neopelex；Conductive materials are sodium sulphate or sodium chloride；Alkaline solution is ammoniacal liquor or sodium hydroxide.
5. the preparation method of super-hydrophobic-superoleophobic material as claimed in claim 4, it is characterised in that each chemical agent concentration is：
Nickel salt：0.05 ~ 0.15M, mantoquita：0.05 ~ 0.15M, sodium hypophosphite：0.01 ~ 0.05M, citric acid：0.01 ~ 0.10M, surface
Activating agent：0.5 ~ 0.15g/L, conductive materials：0.06~0.12M.
6. the preparation method of super-hydrophobic-superoleophobic material as claimed in claim 1, it is characterised in that：The chain alkyl silica
Alkane reagent is in dodecyltrimethoxysilane, hexadecyl trimethoxy silane and octadecyl trimethoxysilane
Any one or a few mixture.
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| CN108165963A (en) * | 2017-12-11 | 2018-06-15 | 中国工程物理研究院化工材料研究所 | A kind of preparation method to high glutinous complicated liquid phase with lyophoby characteristic surface |
| CN108384443A (en) * | 2018-01-11 | 2018-08-10 | 淮阴工学院 | Hybrid super hydrophobic coating and its preparation method and application |
| CN108441847A (en) * | 2018-05-29 | 2018-08-24 | 上海应用技术大学 | A kind of base steel super hydrophobic surface and preparation method thereof based on Ni-Mo-P chemical depositions |
| CN109351290A (en) * | 2018-12-06 | 2019-02-19 | 中石化炼化工程（集团）股份有限公司 | Prevent backstop, its preparation process and the air inlet feed distributor of slurry oil adverse current |
| CN109402693A (en) * | 2018-10-25 | 2019-03-01 | 浙江大学 | Load the Preparation method and use of the mesoporous silicon oxide based superhydrophobic thin films of corrosion inhibiter |
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| US11708494B2 (en) | 2020-02-14 | 2023-07-25 | Icp Construction, Inc. | Oleophobic and hydrophobic composition |
| CN111534841A (en) * | 2020-04-14 | 2020-08-14 | 北京航空航天大学 | Reversible wetting of electric field induced liquid metal on metal substrate and application |
| CN111534841B (en) * | 2020-04-14 | 2021-07-30 | 北京航空航天大学 | Reversible wetting of electric field induced liquid metal on metal substrate and application |
| CN112982020A (en) * | 2021-03-22 | 2021-06-18 | 中国石油大学(华东) | Preparation method of high-strength and high-efficiency oil-water separation filter paper |
| CN112982020B (en) * | 2021-03-22 | 2022-04-15 | 中国石油大学(华东) | Preparation method of high-strength and high-efficiency oil-water separation filter paper |
| CN115029746A (en) * | 2022-07-21 | 2022-09-09 | 中国科学院宁波材料技术与工程研究所 | SLIPS surface coating suitable for multiple metal substrates and preparation method and application thereof |
| CN115029746B (en) * | 2022-07-21 | 2024-03-26 | 中国科学院宁波材料技术与工程研究所 | SLIPS surface coating applicable to various metal substrates, and preparation method and application thereof |
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