CN108796583B - A kind of preparation method of the super-hydrophobic passivating film of Pure Iron Surface corrosion resistance - Google Patents

A kind of preparation method of the super-hydrophobic passivating film of Pure Iron Surface corrosion resistance Download PDF

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Publication number
CN108796583B
CN108796583B CN201810675942.8A CN201810675942A CN108796583B CN 108796583 B CN108796583 B CN 108796583B CN 201810675942 A CN201810675942 A CN 201810675942A CN 108796583 B CN108796583 B CN 108796583B
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super
electrolyte
pure iron
passivating film
hydrophobic
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CN108796583A (en
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金洙吉
范康男
郭江
朱祥龙
王泽北
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Dalian University of Technology
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Dalian University of Technology
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/34Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2518/00Other type of polymers
    • B05D2518/10Silicon-containing polymers

Abstract

The invention belongs to super-hydrophobic film layer preparation technical fields, a kind of preparation method of super-hydrophobic passivating film of Pure Iron Surface corrosion resistance is provided, the method that this method passes through electrochemical corrosion, using specific electrolyte, the passivating film of one layer of high impedance is generated in iron surface, super-hydrophobicity is showed after silicon fluoride is modified, wherein machined parameters are as follows: initial current density is 0.1~20A/cm2, 2~50m/s of electrolyte flow rate;Process time 5s~1000s.Electrolyte used in preparation process of the present invention is at low cost; environmentally friendly and preparation process is simple; the passivating film prepared super-hydrophobicity with higher under silicon fluoride modification; contact angle can reach 160 °; roll angle is up to 2.1 °; the passivating film can make the corrosion potential of workpiece surface shuffle about 0.19V simultaneously, play a very good protection to pure iron matrix.

Description

A kind of preparation method of the super-hydrophobic passivating film of Pure Iron Surface corrosion resistance
Technical field
The invention belongs to super-hydrophobic film layer preparation technical fields, are related to one kind and are used to prepare the super-hydrophobic passivating film of corrosion resistance The formula of electrolyte and its preparation method of the super-hydrophobic film.
Background technique
Ingot iron has many advantages, such as that saturation induction density is high, coercivity is low, magnetic conductivity is high, cold and hot working performance is good, It is used widely in the industry such as electric appliance, telecommunication, electronics, aviation.However pure iron is due to its active chemical property, in humidity And be easily corroded in water environment, to restrict its application prospect.
With the development of technology, for iron material and ferrous alloy, researcher proposes a variety of microstructure buildings Method.Such as document Fan Y, He Y, Luo P, et al.A facile electrodeposition process to fabricate corrosion-resistant superhydrophobic surface on carbon steel[J] .Applied Surface Science, 2016,368:435-442. and number of patent application be 201610946822.8 and 201710192543.1 deposit microstructure layer on ferrous alloy surface using electrochemistry, chemical deposition respectively, but a large amount of The use of chemical reagent not only increases cost, while causing pollution to environment again.Number of patent application 201610017219.1 The structure sheaf of asperity is provided in workpiece surface corrosion by chemical dissolution method, however spray time is too long, and needs Peripheral equipment is needed to do protective treatment.Number of patent application be 201510012667.8 by way of electrochemical dissolution in table Micro-nano dual asperity structure out is corroded in face, and by having superhydrophobic property after surface modification, but this method uses chemistry examination Agent is not only various, and to staff, there are security risks for the use of strong acid and strong base, also unfriendly to environment.Therefore, one is developed Kind is simple, method efficiently, safe prepares corrosion resistance super hydrophobic surface on Pure Iron Surface is particularly important.
Summary of the invention
For the deficiencies in the prior art, the present invention provides a kind of side for preparing super-hydrophobic film layer simple to operation Method, the super-hydrophobic film layer corrosion resistance with higher being prepared.
In order to achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of preparation method of the super-hydrophobic passivating film of Pure Iron Surface corrosion resistance, this method are based on anode oxidation film-forming skill Art, using specific electrolyte, generates the passivating film of one layer of high impedance in iron surface, by fluorine by the method for electrochemical corrosion Super-hydrophobicity is showed after hydride modified.Specifically includes the following steps:
(1) electrolyte is configured
At room temperature, sodium molybdate, sodium chloride are added in deionized water, magnetic agitation 5~10min latter two electrolyte is abundant Dissolution is uniformly mixed, and obtains electrolyte.Sodium molybdate, the 0.1~5g of 0.5~10g are added in every 1000ml deionized water Sodium chloride.
(2) ingot iron (DT4E) is used as basis material, it is spare using alcohol, distilled water ultrasonic cleaning drying respectively.
(3) pure iron connect with pulse power anode and does anode, and cathode plate face needs to prepare super-hydrophobic antisepsis erosion film layer Surface is processed, and the cation for dissolving Pure Iron Surface reacts generation high impedance film with the molybdate in electrolyte and is attached to work On part surface.The technological parameter of processing are as follows: initial current density is 0.1~20A/cm2, duty ratio 10~100%, frequency 1~ 50kHz, electrolyte flow rate: 2~50m/s;Process time: 5s~1000s.
(4) it dries up, and places sufficiently de- in dry environment after rinsing the film layer after step (3) processing using deionized water Water.
(5) the sufficiently dewatered workpiece of step (4) is immersed in the silicon fluoride ethanol solution that mass fraction is 1% to modify and is dropped Low-surface-energy is finally dried, and Pure Iron Surface obtains the super-hydrophobic passivating film of corrosion resistance.
Compared with prior art, beneficial achievement of the invention is as follows:
(1) while having superhydrophobic property, with the increase of thicknesses of layers, the corrosion potential on surface is gradually shuffled, Show that its corrosion resistance is gradually improved.
(2) electrolyte used in is at low cost, environmentally friendly, and preparation process is simple;The passivating film prepared exists Silicon fluoride modification is lower to have super-hydrophobicity, and contact angle can reach 160 °, and roll angle is up to 2.1 °, while after obtaining anodic passivity film Phase just has corrosion resistance without extra process, which can make the corrosion potential of workpiece surface shuffle about 0.19V, to pure Iron matrix plays a very good protection.
Detailed description of the invention
Fig. 1 is the contact angle of super hydrophobic surface obtained by present example.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Using alcohol distillation water be cleaned by ultrasonic pure iron matrix and dry up it is spare, with beaker measure 1000ml deionized water, Enter in electrolytic cell, successively weigh sodium molybdate 5g, sodium chloride 1g, in the case where constantly being stirred using magnetic stirrer, is added step-wise to It is sufficiently stirred in deionized water 5 minutes, so that solute is sufficiently dissolved mixing, obtain electrolyte.
Pure iron is connect with positive pole does anode, and copper sheet faces Pure Iron Surface to be processed as cathode, and initial current is close Degree is 1.1A/cm2, duty ratio 50%, frequency 10kHz, electrolyte flow rate 12.5m/s, process time 60s.
Mass fraction is immersed in after pure iron sufficiently to be dried up to dehydration to reduce surface in 1% silicon fluoride ethanol solution Can, finally dry.After using the modification of 1% silicon fluoride ethanol solution, super-hydrophobicity is presented in surface.
The anodic passivity film contact angle that the present invention is prepared is about 161 °, and roll angle is about 2.1 °, and current potential is relative to original The current potential on beginning surface shuffles about 0.19V.
Embodiments of the present invention above described embodiment only expresses, but it cannot be understood as special to the present invention The limitation of the range of benefit, it is noted that for those skilled in the art, without departing from the inventive concept of the premise, Various modifications and improvements can be made, these are all belonged to the scope of protection of the present invention.

Claims (2)

1. a kind of preparation method of the super-hydrophobic passivating film of Pure Iron Surface corrosion resistance, which is characterized in that pass through electrochemical corrosion Method is generated the passivating film of one layer of high impedance in iron surface, is showed after silicon fluoride is modified super-hydrophobic using specific electrolyte Property;Preparation method specifically includes the following steps:
(1) electrolyte is configured
At room temperature, sodium molybdate, sodium chloride are added in deionized water, magnetic agitation latter two electrolyte is sufficiently dissolved, mixed It is even, obtain electrolyte;The sodium molybdate of 0.5~10g, the sodium chloride of 0.1~5g are added in every 1000ml deionized water;
(2) it using ingot iron as basis material, is dried up after ultrasonic cleaning spare;
(3) pure iron connect with pulse power anode and does anode, and cathode plate face needs to prepare the surface of super-hydrophobic antisepsis erosion film layer It is processed, the cation for dissolving Pure Iron Surface reacts generation high impedance film with the molybdate in electrolyte and is attached to workpiece table On face;The technological parameter of processing are as follows: initial current density is 0.1~20A/cm2, duty ratio 10~100%, frequency 1~ 50kHz, electrolyte flow rate: 2~50m/s;Process time: 5s~1000s;
(4) it is dried up after rinsing the film layer after step (3) processing using deionized water, and places in dry environment and be sufficiently dehydrated;
(5) the sufficiently dewatered workpiece of step (4) is immersed into modification drop low-surface-energy, pure iron after drying in silicon fluoride ethanol solution Surface obtains the super-hydrophobic passivating film of corrosion resistance.
2. a kind of preparation method of super-hydrophobic passivating film of Pure Iron Surface corrosion resistance according to claim 1, feature exist In the mass fraction of silicon fluoride ethanol solution is 1% in the step (4).
CN201810675942.8A 2018-06-27 2018-06-27 A kind of preparation method of the super-hydrophobic passivating film of Pure Iron Surface corrosion resistance Active CN108796583B (en)

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CN114717619B (en) * 2022-04-07 2024-04-02 中国科学院青海盐湖研究所 Method for preparing super-hydrophobic film by utilizing nickel-iron alloy one-step electrolytic deposition

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101020810A (en) * 2007-02-14 2007-08-22 天津大学 Water-base grinding fluid for on-line electrolytic grinding
CN104846376A (en) * 2015-05-29 2015-08-19 清华大学 Preparation method of metal-based super-hydrophobic surface

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101020810A (en) * 2007-02-14 2007-08-22 天津大学 Water-base grinding fluid for on-line electrolytic grinding
CN104846376A (en) * 2015-05-29 2015-08-19 清华大学 Preparation method of metal-based super-hydrophobic surface

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