CN104911644B - The preparation method of super-hydrophobic zinc coat on a kind of steel surface - Google Patents
The preparation method of super-hydrophobic zinc coat on a kind of steel surface Download PDFInfo
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- CN104911644B CN104911644B CN201510178128.1A CN201510178128A CN104911644B CN 104911644 B CN104911644 B CN 104911644B CN 201510178128 A CN201510178128 A CN 201510178128A CN 104911644 B CN104911644 B CN 104911644B
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Abstract
The invention discloses a kind of preparation methods of super-hydrophobic zinc coat on steel surface, belong to electrodeposition.Steel matrix is put into the zinc sulfate solution without smoothing agent and brightener carries out two step electrodeposition process first by the present invention: the first step, which is electrodeposited on steel matrix surface, obtains larger-size coarse structure, second step has obtained the relatively small fine structure of size on the basis of being electrodeposited in larger-size micro-structure, and then forms micro-nano coarse structure；Then the steel curved beam for containing micro-nano coarse structure zinc coat to this carries out fluorination treatment to reduce its surface energy, obtains super hydrophobic functional surface.The contact angle of distilled water and the function surface is more than 150 °, and roll angle has reached super-hydrophobicity less than 10 °.This super-hydrophobic Several Thiourea Derivatives on Zinc Plate Surface not only has the corrosion resistance of traditional zinc coat while having self-cleaning property, opens a new application field for electrodeposition technology.This method is easily operated, cheap, and base shape is unrestricted, use easy to spread.
Description
Technical field
The present invention relates to a kind of preparation methods of super-hydrophobic zinc coat on steel surface, and in particular to two step of steel matrix surface
Electrodeposition process and low energy modification, and then realize the super-hydrophobicity of steel surface.
Background technique
Found from the secret of " lotus leaf effect " by some researchers, super-hydrophobicity cause the great interest of people and extensively
Concern, and super hydrophobic surface plays an important role in daily life and industrial and agricultural production, such as: having hydrophobic meal
Tool, textile, ship, solar panel etc..For this purpose, more and more people start to probe into various methods to prepare super-hydrophobic table
Face, and discovery prepare super hydrophobic surface method key factor be two kinds: one is improve hydrophobic material surface roughness,
Another kind is to carry out low energy modification to the surface with coarse structure, wherein the latter is the most commonly used method.
There are much reports about method for preparing super-hydrophobic surface at present.But the matrix that most methods are related to
For a few materials such as cotton fiber, glass, silicon wafer, magnesium and magnesium alloy, aluminium and aluminium alloy, the preparation phase of super hydrophobic surface in steel matrix
To less.In addition, many preparation methods, such as orientation etching, gas/liquid mutually deposit, mould plate technique, collosol and gel, there is preparation
The problems such as condition harshness, required higher cost, the popularization and large area for limiting these methods use.
Traditional electrodeposition technology is mostly the appearance for improving basis material, assigns material surface certain physical chemistry
Energy is equal, is formed by surface and requires smooth greatly.Super hydrophobic surface usually requires micro-nano coarse structure, so, electricity
Smoothing agent and brightener are not added in plating solution and contributes to form fine coarse structure instead.In addition, different electrodeposition technologies is joined
Number can obtain different surface micro-structures.Zinc provides machine to parent metal usually as the anodic coating of some metal materials
Tool protection and electrochemical protection.If preparing super hydrophobic surface on zinc coat, obtained super hydrophobic surface not only has anti-corrosion
Property, while also there is certain self-cleaning property, the application range of meeting further expansion electroplated layer.Nano-plating ([day] , Du side
Rut, Chemical Industry Press, 2006,9) pattern of Several Thiourea Derivatives on Zinc Plate Surface under different electro-deposition parameters is reported, and obtain: electro-deposition
Time extends (coating is thicker), and the micro-bulge of coating is thicker.Therefore, micron and nanometer composite structure is realized with two step electro-deposition:
One step forms larger-size micro-structure using the electro-deposition of long period, and second step is original using being electrodeposited in for short period
The lesser micro-structure of size is formed in larger-size micro-structure.
The present invention constructs micro nano structure on steel matrix surface by simple two steps electrodeposition process, and repairs in conjunction with low energy
Decorations form super hydrophobic surface.This surface not only has corrosion resistance, while also having certain self-cleaning property, and technical process letter
Single, at low cost, practicability is stronger, suits large area to popularize.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of super-hydrophobic zinc coat on simple steel surface.
Super hydrophobic functional surface in steel matrix of the present invention is realized jointly by two step electro-deposition zinc layers and low energy modification.
The preparation method of super-hydrophobic zinc coat on a kind of steel surface, it is characterised in that this method successively includes following
Step:
1) successively with the metallographic liquid honing steel curved beam surface of 600#-2000# to smooth, with improve electro-deposition zinc layers with
The binding force on steel matrix surface is cleaned by ultrasonic and dry, while zinc sample is also successively beaten with the metallographic waterproof abrasive paper of 600#-2000#
Surface is ground to smooth；
2) oil removing 15min (60 DEG C), then the pickling work in pickling solution in alkali wash water by the good steel curved beam of above-mentioned polishing
Change 10s (room temperature), is quickly rinsed and dried with a large amount of clear water；
3) steel curved beam of above-mentioned acid-wash activation be cathode, the pure zine plate polished be anode, in zinc sulfate solution into
Two step electro-deposition of row, obtains micro-nano coarse structure surface, sees Fig. 1；
4) steel curved beam containing coarse structure zinc coat is put into perfluoro caprylic acid ethanol solution and impregnates a timing
Between, it is put into culture dish after taking-up, dries to obtain super hydrophobic surface at room temperature.
5) steel curved beam used in step 1) is X90 pipe line steel；
6) alkali wash water used in step 2) is NaOH (30g/L), Na2CO3(20g/L)、Na3PO4(20g/L) and Na2SiO3
The mixed aqueous solution of (10g/L) composition；Pickling solution is the H that volume fraction is 10%2SO4Aqueous solution；
7) electroplate liquid described in step 3) is the ZnSO of 180-260g/L4﹒ 7H2(volume fraction is 10% to O aqueous solution
H2SO4The pH ≈ 4 for adjusting electroplate liquid, without smoothing agent and brightener)；
8) electroplating technological parameter described in step 3) is as follows: temperature of electroplating solution is 15-75 DEG C；The electric current of first step electro-deposition
Density is 2-6A/dm2, electrodeposition time 15-40min；After reaching the time set, electric current is quickly adjusted to 9-11A/
dm2Carry out second step electro-deposition, electrodeposition time 1-20min；Surface quickly is washed off with a large amount of clear water after reaction
Residual liquid and drying；
9) concentration of the perfluoro caprylic acid dehydrated alcohol described in step 5) is 0.005-0.02mol/L, soaking time 3-
13 days.
The present invention is electrodeposited in steel surface by the first step and forms larger-size coarse structure, then passes through second step
It is electrodeposited on the basis of original micro-structure and forms the relatively small coarse structure of size, to constitute micron and nanometer composite structure；
Low energy modification finally is carried out with perfluoro caprylic acid ethanol solution, obtains super hydrophobic surface.Distilled water is dripped to the steel handled
The contact angle of surface progress contact angle determination, this surface and water is greater than 150 °.
The invention has the following advantages that
1) method used in is traditional electrodeposition technology, and required equipment price is cheap, to the shape and size of sample
There is no particular/special requirement；
2) raw material is cheap and easily-available.Using steel as raw material, is modified by two step electro-deposition and low energy, prepare super hydrophobic surface；
3) all technical process all carry out in the solution, and easy to operate, suit large area to popularize；
4) super hydrophobic surface obtained by also extends to other metal surfaces, thus the scope of application it is relatively wide, in industry and
It has broad application prospects in life.
Detailed description of the invention
The present invention will be further explained below with reference to the attached drawings.
Fig. 1 is the SEM photograph of the super-hydrophobic zinc coat of X90 pipe line steel in the embodiment of the present invention；
Fig. 2 is contact angle of the water droplet on the super-hydrophobic Several Thiourea Derivatives on Zinc Plate Surface of X90 pipe line steel, and size is 152.36 °.
Specific embodiment
The present invention will be further explained with reference to the examples below, as described below, is only to preferable implementation of the invention
Example, not limits the present invention, any person skilled in the art is possibly also with the disclosure above
Technology contents be changed to the equivalent embodiment changed on an equal basis.Without departing from the concept of the present invention, according to the present invention
Technical spirit any simple modification made to the above embodiment or equivalent variations, fall within the scope of protection of the present invention.
The preparation method of super-hydrophobic zinc coat on a kind of steel surface, is specifically completed by following steps:
1, with the smooth X90 pipe line steel of the metallographic liquid honing of 600#-2000# and pure zine plate specimen surface, then distinguish
Acetone, dehydrated alcohol, distilled water are cleaned by ultrasonic 5 minutes and drying；
2, the pipe line steel specimen surface for not needing plating is sticked with insulating tape, and steel curved beam is successively then carried out to alkali cleaning and is removed
Oily 15min (60 DEG C, the Na of NaOH, 20g/L of 30g/L2CO3, 20g/L Na3PO4, 10g/L Na2SiO3The mixing water of composition
Solution), acid-wash activation 10s (room temperature, volume fraction be 10% H2SO4), simultaneously rapid draing is washed with a large amount of clear water after taking-up；
3, the above-mentioned pipeline steel curved beam handled well is cathode, and pure zine plate is anode, in the ZnSO of 240g/L4﹒ 7H2O aqueous solution
In (volume fraction be 10% H2SO4Adjust the pH ≈ 4 of electroplate liquid) it is electroplated, temperature of electroplating solution is 25 DEG C, and current density is
4A/dm2, electric current is quickly adjusted to 9A/dm after reaching the time set by electrodeposition time 30min2Carry out second step electricity
Deposition, electrodeposition time 3min；Remained on surface liquid and drying quickly are washed off with a large amount of clear water after reaction；Its table
Micro-nano coarse structure is presented in face pattern, sees Fig. 1；
4, the pipeline steel curved beam that step 3 obtains is put into the perfluoro caprylic acid ethanol solution of 0.01mol/L and is impregnated
It 11 days, is put into culture dish after taking-up, dries to obtain super hydrophobic surface at room temperature.After measured, the surface and distilled water
Static contact angle be 152.36 °, see Fig. 2, and roll angle is less than 10 °.
Claims (1)
1. the preparation method of super-hydrophobic zinc coat on a kind of steel surface, it is characterised in that this method successively includes following two step
It is rapid:
(1) steel polished smooth are successively used as to cathode after alkali cleaning, pickling, using the pure zine plate polished smooth as sun
Pole, in the ZnSO of 180-260g/L4﹒ 7H2Electrodeposition process is carried out in O aqueous solution, it is 10% that volume fraction is used before electro-deposition
H2SO4The pH=4 of electroplate liquid is adjusted, temperature of electroplating solution is 15-75 DEG C, and the current density of first step electro-deposition is 2-6A/dm2, electricity
Sedimentation time is 15-40min, and after reaching setting time, current density is quickly adjusted to 7-11A/dm2, carry out second step electricity
Deposition, electroplating time 1-20min quickly wash off remained on surface liquid and drying with a large amount of clear water after reaction,
The zinc coat of micro-nano coarse structure is obtained on steel surface；
(2) that the steel curved beam containing zinc coat that step (1) obtains is put into 0.005-0.02mol/L perfluoro caprylic acid dehydrated alcohol is molten
It is impregnated 3-13 days in liquid, is put into culture dish after taking-up, dries at room temperature, obtain super hydrophobic surface.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110453257A (en) * | 2019-08-16 | 2019-11-15 | 山东科技大学 | A kind of super-hydrophobic Zn-PTFE composite electrodeposition layer and preparation method |
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| CN105256342B (en) * | 2015-10-19 | 2017-10-20 | 华南理工大学 | A kind of super hydrophobic surface based on copper and preparation method thereof |
| CN105386090B (en) * | 2015-11-09 | 2018-05-11 | 广东工业大学 | A kind of preparation method of the superoleophobic metal surface with indent micropore |
| CN105586616A (en) * | 2016-01-18 | 2016-05-18 | 苏州市华婷特种电镀有限公司 | Process for pretreating part to be plated in electroplating process |
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| CN108301024B (en) * | 2018-02-28 | 2020-04-07 | 北京科技大学 | Method for preparing surface hydrophobic structure coating |
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| CN113215627A (en) * | 2021-05-10 | 2021-08-06 | 中国石油大学(华东) | Method for preparing super-hydrophobic zinc sulfide coating on surface of stainless steel |
| CN114807947B (en) * | 2022-05-23 | 2024-04-12 | 四川晟实科技有限公司 | Preparation method of stainless steel hydrophobic wear-resistant nano film for organic analytical instrument |
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| CN101440510B (en) * | 2007-11-21 | 2010-08-25 | 国家纳米科学中心 | Preparation of super-hydrophobic surface for metal anti-corrosive and self-cleaning effects |
| CN101935859A (en) * | 2010-08-27 | 2011-01-05 | 中国科学院海洋研究所 | Simple and convenient method for preparing super-hydrophobic film on surface of metal matrix |
| CN104195539A (en) * | 2014-08-26 | 2014-12-10 | 中国石油大学(华东) | Reparation method for zinc super-hydrophobic surface |
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