CN108977801A - A kind of preparation method for the 3-D nano, structure plate membrane that high water resistant is anti-corrosion - Google Patents
A kind of preparation method for the 3-D nano, structure plate membrane that high water resistant is anti-corrosion Download PDFInfo
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- CN108977801A CN108977801A CN201810938667.4A CN201810938667A CN108977801A CN 108977801 A CN108977801 A CN 108977801A CN 201810938667 A CN201810938667 A CN 201810938667A CN 108977801 A CN108977801 A CN 108977801A
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- 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
- C23C22/05—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 aqueous solutions
- C23C22/60—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 aqueous solutions using alkaline aqueous solutions with pH greater than 8
- C23C22/62—Treatment of iron or alloys based thereon
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- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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- 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
- C23C22/73—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 characterised by the process
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- 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
- 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
- C23C22/82—After-treatment
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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
- C23F17/00—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
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Abstract
The invention discloses a kind of preparation methods of 3-D nano, structure plate membrane that high water resistant is anti-corrosion, pretreated steel plate is successively constructed into micron octahedral structure, nanoparticle structure and nano bar-shape structure after the processing of hydro-thermal method twice and primary annealing, it is surface modified again with low-surface energy substance and the anti-corrosion 3-D nano, structure plate membrane of high water resistant is prepared, its water repelling property and corrosion resisting property are enhanced, to extend service life.
Description
Technical field
The present invention relates to technical field of metal anti-corrosion, and in particular to a kind of 3-D nano, structure plate membrane that high water resistant is anti-corrosion
Preparation method.
Background technique
Metal erosion either all easily occurs in the industry or in life very much, and steel stand in the breach, as industry
Soul is widely used in every field, annual because economic loss brought by corroding is countless.At present for the anti-of metal
Rotten measure is mainly using corrosion inhibiter, anticorrosive paint etc., corrosion inhibiter less effective in openr large area region, and
Possess good antisepsis in smaller range.Although anticorrosive paint anti-corrosion effect is relatively good, due to price ratio
It is higher but also pollution, the especially heavy metal ion in organic coating to be generated to environment easily strong to human body in use
Health has an impact, to limit its range used.So how the antiseptic property of the raising metal of highly effective and safe green is
Technical problem in the urgent need to address.
Summary of the invention
In order to solve the deficiencies in the prior art, the present invention is by providing a kind of 3-D nano, structure steel plate that high water resistant is anti-corrosion
The preparation method of film, it is therefore an objective to enhance water repelling property and the corrosion resisting property of steel plate to reduce the rate of corrosion, extend its use
Service life.
Specifically, a purpose of the invention is to provide a kind of preparation side of 3-D nano, structure plate membrane that high water resistant is anti-corrosion
Method includes the following steps:
S1, steel plate is pre-processed: naturally dry after cleaning 10~20min with ethyl alcohol and distilled water;
S2, the pretreated steel plate of S1 is successively successively constructed after the processing of hydro-thermal method twice and primary annealing
Steel plate, the steel plate of nanoparticle structure and the steel plate of nano bar-shape structure of micron octahedral structure, then use low-surface energy substance
It is surface modified and the anti-corrosion 3-D nano, structure plate membrane of high water resistant is prepared;Specific step is as follows:
Steel plate is carried out the step of first time hydro-thermal method is handled by S21 are as follows:
The ethylenediamine solution that 15~20ml concentration is 3.7~3.75mol/L is prepared, ethylenediamine solution and steel plate are all put into
In reaction kettle, 160~165 DEG C are heated to, 6~7h is reacted, is cleaned and dried with ethyl alcohol and distilled water after cooled to room temperature,
Obtain the steel plate of micron octahedral structure;
Steel plate is carried out the step of second of hydro-thermal method is handled by S22 are as follows:
The steel plate of micron octahedral structure is placed again into reaction kettle, and be added thereto by inorganic alkali solution and
FeCl3The mixed liquor of solution composition is heated to 90~95 DEG C, reacts 3~4h, is cleaned after being cooled to room temperature with ethyl alcohol and distilled water
And dry, obtain the steel plate of nanoparticle structure;Wherein, the volume of the mixed liquor is 20~25ml, the inorganic alkali solution
Amount concentration be 0.05~0.3mol/L, the FeCl3The amount concentration of solution is 0.01~0.02mol/L;
S23, will by hydro-thermal method twice treated steel plate made annealing treatment the step of are as follows:
The steel plate of nanoparticle structure is put into annealing furnace and is made annealing treatment, is risen in air atmosphere or oxygen atmosphere
To 530~580 DEG C, anneal temperature 2~2.5h, takes out after its natural cooling, obtains the steel plate of nano bar-shape structure;
S24, the step of being surface modified with low-surface energy substance are as follows:
The steel plate of nano bar-shape structure is put into the low-surface energy substance solution of 6~8mmol/L, wherein solvent is second
Alcohol impregnates 4.5~5.5h at 20~25 DEG C, and taking-up ethyl alcohol and distilled water, which are cleaned and dried, after the completion can be obtained three wieners
Rice structural steel and iron film.
Preferably, the low-surface energy substance is one of stearic acid, myristic acid or octadecylamine.
Preferably, the inorganic alkali solution is NaOH solution.
Compared with prior art, the beneficial effects of the present invention are:
1) the present invention provides a kind of preparation methods of 3-D nano, structure plate membrane that high water resistant is anti-corrosion, use to steel plate
Hydro-thermal method processing method is simple, it is only necessary to which the simple operations such as heating immersion can be completed, and make annealing treatment energy secure surface structure, make
It goes out occurrence structure and forms micro nano structure, then enhances its water repelling property and corrosion resisting property using low-surface energy substance modification.
In addition, stearic acid also can apply to the fields such as food additives and cosmetics, use is safe and secure, as low-surface-energy activity
Agent has safe and non-toxic and environmental pollution small using micro.
2) technology path used in the present invention is very simple, can enhance its water repelling property, water droplet is made to be not easy to be trapped in
Surface of steel plate avoids water droplet from being detained bring oxidation for a long time, it is made to aoxidize surface of steel plate to bring to form corrosion.It removes
Except this, corrosion rate can also be slowed down, not only there is certain anti-corrosion effect to neutral solution, it is molten to acid solution and alkalinity
Liquid also has certain anti-corrosion effect, enhances its corrosion resisting property, to extend service life, reduces corruption to a certain extent
Bring economic loss is lost, and the technology path used is simple, it is easy to accomplish.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is the process flow chart of the embodiment of the present invention 1;
Fig. 2 is 1 water droplet of the embodiment of the present invention on the anti-corrosion 3-D nano, structure plate membrane of the high water resistant that preparation is completed
Contact angle (a) and roll angle (b);
Fig. 3 is wellability (a) of 1 water droplet of the embodiment of the present invention on untreated steel plate, and water droplet is anti-corrosion in high water resistant
3-D nano, structure steel plate on water bullet (b), water jet (c), automatically cleaning (d), impregnate (e);
Fig. 4 is that 1 microstructure product X RD of the embodiment of the present invention analyzes map;
Fig. 5 is the untreated N80 steel (a) of the embodiment of the present invention 1, the 3-D nano, structure steel that high water resistant that treated is anti-corrosion
Plate (b), the micromorphology (c) for the 3-D nano, structure plate membrane that high water resistant is anti-corrosion, the micromorphology under high power lens
(d);
Fig. 6 is N80 steel plate and treated polarization curve of the steel plate in 5wt%NaCl solution in the embodiment of the present invention 1
Scheme (a) and impedance spectrum (b);
Fig. 7 be in the embodiment of the present invention 1 N80 steel plate and treated steel plate in the H of pH=12SO4Polarization in solution is bent
Line chart (a) and impedance spectrum (b);
Polarization of the steel plate in the NaOH solution of pH=14 is bent with treated for N80 steel plate in the embodiment of the present invention 1 by Fig. 8
Line chart (a) and impedance spectrum (b).
Specific embodiment
In order to enable those skilled in the art to more fully understand, technical solution of the present invention is practiced, below with reference to specific
The invention will be further described for embodiment, but illustrated embodiment is not as a limitation of the invention.
Unless otherwise defined, the hereinafter used all technical terms for being and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection scope.Unless otherwise specified, it the various raw materials used in the following embodiment of the present invention, reagent, instrument and sets
It is standby to be commercially available by market or be prepared by existing method.
1-8 with reference to the accompanying drawing, specific embodiments of the present invention will be described in detail, it is to be understood that of the invention
Protection scope is not limited by the specific implementation.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.
Following example provides a kind of system of 3-D nano, structure plate membrane that high water resistant is anti-corrosion by taking N80 steel plate as an example
Preparation Method carries out specific for example, wherein Fig. 1 is easy preparation flow of the invention to technical solution of the present invention
Figure, the present invention are to prepare one layer of water resistant corrosion-resisting film in surface of steel plate to reduce the area contacted with water to reach water resistant and anti-corrosion
Effect, microstructure in steel surface is mainly prepared by hydro-thermal method twice and annealing, finally passes through immersion again
Mode in one layered low-surface energy substance of surface modification.
Embodiment 1
A kind of preparation method for the 3-D nano, structure plate membrane that high water resistant is anti-corrosion of the present embodiment, comprising the following steps:
Steel plate is pre-processed, naturally dry after cleaning 10min with ethyl alcohol and distilled water, preparing 20ml concentration is
Ethylenediamine solution and steel plate are all put into reaction kettle by the ethylenediamine solution of 3.75mol/L, are heated to 165 DEG C, react 7h, from
It is cleaned and is dried with ethyl alcohol and distilled water after being so cooled to room temperature;Then the steel plate handled well is placed again into reaction kettle, is added
Enter NaOH the and 0.01mol/L FeCl that 20ml concentration is 0.2mol/L3The mixed solution of solution is heated to 90 DEG C, reacts 4h,
It is cleaned and is dried with ethyl alcohol and distilled water after being cooled to room temperature;Will treated that steel plate is put into annealing furnace makes annealing treatment,
550 DEG C are warming up in air atmosphere, anneal 2h, takes out after its natural cooling, is then placed in the stearic acid ethyl alcohol of 8mmol/L
In solution, 5h is impregnated at 25 DEG C, taking-up ethyl alcohol and distilled water are cleaned and dried after the completion.
The 3-D nano, structure plate membrane that we are anti-corrosion to the high water resistant prepared in embodiment 1 is tested for the property, and is passed through
Contact angle test proves that it has good water repelling property, and the optical imagery of contact angle is as shown in Fig. 2, its contact angle can achieve
160 ° or so, roll angle can achieve 3.3 ° or so, and when contact angle is greater than 150 ° and roll angle is less than 10 °, performance excess of export is dredged
Aqueous energy, it is seen that prepared water-repellent film has good hydrophobic performance.
Fig. 3 is that water droplet is different on untreated steel plate and the anti-corrosion 3-D nano, structure steel plate of processed high water resistant
Infiltration behavior.Fig. 3 a is wellability of the water droplet on untreated steel plate.It can be seen that water droplet drippage is directly flat on the steel plate
It lies prone on the steel plate, jet stream also will appear on the steel plate to be packed together.And it can be seen that water droplet is dropped in highly resistance from Fig. 3 b-c
When on the 3-D nano, structure steel plate that water is anti-corrosion can nature flick, when water jet on it when also directly can leave table at water beam
Face.Fig. 3 d is demonstrated by the self-cleaning property of the anti-corrosion 3-D nano, structure steel plate of high water resistant, and surface is chalk bits, can band when water drips
Walk the chalk bits on surface.Fig. 3 e is that the anti-corrosion 3-D nano, structure steel plate of high water resistant is immersed directly in water, it can be seen that whole
A surface of steel plate all can form a bright surface, and not any defect is presented on its surface, is said by water to arranging
The anti-corrosion 3-D nano, structure plate membrane of the high water resistant is illustrated to complete that defect is not present.
Fig. 4 is XRD diagram of the anti-corrosion 3-D nano, structure plate membrane of prepared high water resistant after having constructed microstructure
Spectrum, it can be found that the corresponding substance of processed plate membrane is Fe from figure3O4And Fe2O3Two kinds of substances compare Fe3O4(JCPDS
card No.19-0629)Fe2O3Other no extra mutually presence known to the standard PDF of (JCPDS card No.33-0664),
Know that preparation gained film is Fe2O3/Fe3O4Composite film.
The pictorial diagram and its surface microscopic knot of Fig. 5 untreated steel plate and the anti-corrosion 3-D nano, structure steel plate of high water resistant
Structure.Can see steel plate from Fig. 5 a-b, very big change has occurred in rear surface before treatment, and color and structure all exist certain
Difference.It can be seen that there is the micron-sized octahedral structure of some larger sizes from Fig. 5 c, following closely is some granular thereon
Substance appears on octahedra surface.From Fig. 5 c it is found that being the discovery that micron order octahedron under high power lens all is some nanoscales
Particulate material, in addition there are also some rodlike substances attachments on the surface thereof, forms polynary micro/nano level structure, root
Make water droplet on the surface thereof can be by air it is found that this micro/nano level structure can store a large amount of air according to Cassie theory
Completely cut off, shows good water repelling property.
Fig. 6 is polarization curve and resistance of the anti-corrosion 3-D nano, structure plate membrane of high water resistant in the NaCl solution of 5wt%
Anti- map.It can be seen that, relative to untreated steel plate, processed steel plate curve deviates to the left from Fig. 6 a polarization curve,
Corrosion electric current density becomes smaller about 14.4 μm of cm-2, 1 order of magnitude is reduced, corrosion rate is reduced.From Fig. 6 b impedance spectrum
Know that semicircle arc dia significantly increases, in addition RctFor more untreated steel plate, nearly 48 times are increased, improves it in neutrality
Corrosion resistance in salting liquid.
Fig. 7 is H of the anti-corrosion 3-D nano, structure plate membrane of high water resistant in pH=12SO4Polarization curve and resistance in solution
Anti- map.It can be seen that, relative to untreated steel plate, processed steel plate curve also deviates to the left from Fig. 7 a polarization curve,
But offset is less, and corrosion electric current density becomes smaller about 1229.4 μm of cm-2, the corrosion electric current density of untreated steel plate
For 1996.8 μm of cm-2.Increase from the semicircle arc dia of impedance diagram known to Fig. 7 b impedance spectrum, RctMore untreated steel plate
For also increase with it, illustrate which raises corrosion resistances in an acidic solution.
Fig. 8 is polarization curve and resistance of the anti-corrosion 3-D nano, structure plate membrane of high water resistant in the NaOH solution of pH=14
Anti- map.It can be seen that, relative to untreated steel plate, processed steel plate curve also occurs to the left from Fig. 8 a polarization curve
Offset, corrosion electric current density become smaller about 10.5 μm of cm-2, the corrosion electric current density of untreated steel plate is 45.9 μm
cm-2.Increase from the semicircle arc dia of impedance diagram known to Fig. 8 b impedance spectrum, RctAlso increase for more untreated steel plate, says
The bright corrosion resistance which raises in alkaline solution.
Fig. 5 is combined to analyze from Fig. 2-3 it is found that the plate membrane has good hydrophobic performance.From the polarization curve of Fig. 6-8 and
Impedance spectrum illustrates that the plate membrane has it is found that either corrosion resistance is all improved under acid, neutral or alkaline condition
There is good corrosion resisting property.In conclusion the plate membrane has the anti-corrosion 3-D nano, structure performance of good high water resistant.
Embodiment 2
A kind of preparation method for the 3-D nano, structure plate membrane that high water resistant is anti-corrosion of the present embodiment, comprising the following steps:
Steel plate is pre-processed, naturally dry after cleaning 10min with ethyl alcohol and distilled water, preparing 20ml concentration is
Ethylenediamine solution and steel plate are all put into reaction kettle by the ethylenediamine solution of 3.75mol/L, are heated to 160 DEG C, react 6h, from
It is cleaned and is dried with ethyl alcohol and distilled water after being so cooled to room temperature;Then the steel plate handled well is placed again into reaction kettle, is added
Enter NaOH the and 0.01mol/L FeCl that 20ml concentration is 0.05mol/L3The mixed solution of solution is heated to 90 DEG C, reacts 4h,
It is cleaned and is dried with ethyl alcohol and distilled water after being cooled to room temperature;Will treated that steel plate is put into annealing furnace makes annealing treatment,
550 DEG C are warming up in oxygen atmosphere, anneal 2h, takes out after its natural cooling, is then placed in the stearic acid ethyl alcohol of 8mmol/L
In solution, 5h is impregnated at 25 DEG C, taking-up ethyl alcohol and distilled water are cleaned and dried after the completion.
Embodiment 3
A kind of preparation method for the 3-D nano, structure plate membrane that high water resistant is anti-corrosion of the present embodiment, comprising the following steps:
Steel plate is pre-processed, naturally dry after cleaning 10min with ethyl alcohol and distilled water, preparing 20ml concentration is
Ethylenediamine solution and steel plate are all put into reaction kettle by the ethylenediamine solution of 3.75mol/L, are heated to 165 DEG C, react 6h, from
It is cleaned and is dried with ethyl alcohol and distilled water after being so cooled to room temperature;Then the steel plate handled well is placed again into reaction kettle, is added
Enter NaOH the and 0.01mol/L FeCl that 20ml concentration is 0.3mol/L3The mixed solution of solution is heated to 90 DEG C, reacts 4h,
It is cleaned and is dried with ethyl alcohol and distilled water after being cooled to room temperature;Will treated that steel plate is put into annealing furnace makes annealing treatment,
550 DEG C are warming up in air atmosphere, anneal 2h, takes out after its natural cooling, is then placed in the stearic acid ethyl alcohol of 8mmol/L
In solution, 5h is impregnated at 20 DEG C, taking-up ethyl alcohol and distilled water are cleaned and dried after the completion.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.Embodiment described above is only to absolutely prove the present invention
And the preferred embodiment lifted, protection scope are without being limited thereto.Those skilled in the art institute on the basis of the present invention
The equivalent substitute or transformation of work, within the scope of the present invention, protection scope of the present invention is subject to claims.
Claims (3)
1. a kind of preparation method for the 3-D nano, structure plate membrane that high water resistant is anti-corrosion, which comprises the steps of:
S1, steel plate is pre-processed: naturally dry after cleaning 10~20min with ethyl alcohol and distilled water;
S2, the pretreated steel plate of S1 is successively successively constructed into micron after the processing of hydro-thermal method twice and primary annealing
The steel plate of the steel plate of octahedral structure, the steel plate of nanoparticle structure and nano bar-shape structure, then carried out with low-surface energy substance
The anti-corrosion 3-D nano, structure plate membrane of high water resistant is prepared in surface modification;Specific step is as follows:
Steel plate is carried out the step of first time hydro-thermal method is handled by S21 are as follows:
The ethylenediamine solution that 15~20ml concentration is 3.7~3.75mol/L is prepared, ethylenediamine solution and steel plate are all put into reaction
In kettle, 160~165 DEG C are heated to, 6~7h is reacted, is cleaned and dried with ethyl alcohol and distilled water after cooled to room temperature, obtain
The steel plate of micron octahedral structure;
Steel plate is carried out the step of second of hydro-thermal method is handled by S22 are as follows:
The steel plate of micron octahedral structure is placed again into reaction kettle, and is added thereto by inorganic alkali solution and FeCl3Solution
The mixed liquor of composition is heated to 90~95 DEG C, reacts 3~4h, is cleaned and dried with ethyl alcohol and distilled water after being cooled to room temperature, obtained
Obtain the steel plate of nanoparticle structure;Wherein, the volume of the mixed liquor is 20~25ml, and the amount concentration of the inorganic alkali solution is
0.05~0.3mol/L, the FeCl3The amount concentration of solution is 0.01~0.02mol/L;
S23, will by hydro-thermal method twice treated steel plate made annealing treatment the step of are as follows:
The steel plate of nanoparticle structure is put into annealing furnace and is made annealing treatment, is warming up in air atmosphere or oxygen atmosphere
530~580 DEG C, anneal 2~2.5h, takes out after its natural cooling, obtains the steel plate of nano bar-shape structure;
S24, the step of being surface modified with low-surface energy substance are as follows:
The steel plate of nano bar-shape structure is put into the low-surface energy substance solution of 6~8mmol/L, wherein solvent is ethyl alcohol,
4.5~5.5h is impregnated at 20~25 DEG C, taking-up ethyl alcohol and distilled water, which are cleaned and dried, after the completion can be obtained three-dimensional manometer knot
Structure plate membrane.
2. the preparation side for the 3-D nano, structure plate membrane that a kind of high water resistant according to claim 1 is anti-corrosion, feature exist
In the low-surface energy substance is one in stearic acid, myristic acid, octadecylamine or other safe and non-toxic low-surface energy substances
Kind.
3. the preparation side for the 3-D nano, structure plate membrane that a kind of high water resistant according to claim 1 is anti-corrosion, feature exist
In the inorganic alkali solution is NaOH solution.
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CN201810938667.4A CN108977801B (en) | 2018-08-17 | 2018-08-17 | Preparation method of three-dimensional nano-structure steel plate film with high water resistance and corrosion resistance |
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CN110205452A (en) * | 2019-04-24 | 2019-09-06 | 西北大学 | Hydrophobic steel plate of a kind of micron of octahedron/nano whiskers structure and preparation method thereof |
CN113564589A (en) * | 2021-07-05 | 2021-10-29 | 浙江瀛迪新材料科技有限公司 | Steel plate film and production process thereof |
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CN110205452B (en) * | 2019-04-24 | 2020-10-27 | 西北大学 | Hydrophobic steel plate with micron octahedron/nano needle-shaped structure and preparation method thereof |
CN113564589A (en) * | 2021-07-05 | 2021-10-29 | 浙江瀛迪新材料科技有限公司 | Steel plate film and production process thereof |
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