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 PDFInfo
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- 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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- pure iron
- passivating film
- hydrophobic
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 27
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 22
- 230000007797 corrosion Effects 0.000 title claims abstract description 18
- 238000005260 corrosion Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003792 electrolyte Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 16
- 230000004048 modification Effects 0.000 claims abstract description 6
- 238000012986 modification Methods 0.000 claims abstract description 6
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000006056 electrooxidation reaction Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- YSBQKZZHQPPKEL-UHFFFAOYSA-N ethanol;tetrafluorosilane Chemical compound CCO.F[Si](F)(F)F YSBQKZZHQPPKEL-UHFFFAOYSA-N 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 239000011684 sodium molybdate Substances 0.000 claims description 5
- 235000015393 sodium molybdate Nutrition 0.000 claims description 5
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 230000003260 anti-sepsis Effects 0.000 claims description 2
- 150000001768 cations Chemical class 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 230000003628 erosive effect Effects 0.000 claims description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
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
- C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2518/00—Other type of polymers
- B05D2518/10—Silicon-containing polymers
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
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
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).
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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 |
CN116022848A (en) * | 2022-12-06 | 2023-04-28 | 西安诺博尔稀贵金属材料股份有限公司 | By using molybdenum copper alloy scrap production of molybdic acid method for preparing sodium compound |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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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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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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