CN106048665A - Method for preparing metal-base super-oleophobic composite casting layer by using hot compression deformation process - Google Patents
Method for preparing metal-base super-oleophobic composite casting layer by using hot compression deformation process Download PDFInfo
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- CN106048665A CN106048665A CN201610534243.2A CN201610534243A CN106048665A CN 106048665 A CN106048665 A CN 106048665A CN 201610534243 A CN201610534243 A CN 201610534243A CN 106048665 A CN106048665 A CN 106048665A
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- Prior art keywords
- layer
- superoleophobic
- micro
- compression deformation
- hot compression
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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
- C25D1/00—Electroforming
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F5/00—Electrolytic stripping of metallic layers or coatings
Abstract
The invention discloses a method for preparing a metal-base super-oleophobic composite casting layer by using a hot compression deformation process. A compact smooth composite casting layer can be obtained more easily by adopting a composite electroforming technology at appropriate impulse electrical parameters. By adopting different particle sizes of polymers and controlling the temperature and the pressure of a hot plate, a structure having different concave curvature can be obtained, so that a workpiece surface having controllable oleophobic property can be obtained. A technology and equipment that are used in the method are simple; the cost is low; and the method is applicable to super-oleophobic modification on large area metal surfaces.
Description
Technical field
The present invention relates to a kind of method that hot compression deformation method prepares the superoleophobic compound cast layer of Metal Substrate, be used for changing metal watch
Face wettability so that it is there is superoleophobic characteristic.Being applicable to the preparation on the superoleophobic surface of large area, preparation cost is low, easily realizes, and belongs to
In field of electrochemical deposition.
Background technology
Moistening (Wetting) is that solid interface is changed into the phenomenon of solid-liquid interface by solid-air interface.And wettability
(wettability) ability or tendentiousness that a kind of liquid sprawls at a kind of surface of solids are referred to.Wettability is to there is nature
In universal phenomenon, such as rainwater fall to being formed spherical drop after lotus leaf surface and the phenomenon that tumbles and Folium Nelumbinis " go out mud and
Do not contaminate " self_cleaning effect, be super-hydrophobic phenomenon.In addition the many foot of animals and plants such as water skipper, the wing of butterfly, Rice Leafs
Deng, it may have ultra-hydrophobicity.Research shows, the superhydrophobic characteristic that all these surfaces are had is due to micro-nano coarse knot
Structure and low-surface energy substance cooperatively form.
Wettability is also material science and the importance in Surface Engineering field simultaneously, in daily life, commercial production, agriculture
Industry has many important application in producing.So-called super-hydrophobic refer to the water droplet static contact angle at the surface of solids more than 150 °, in like manner,
Superoleophobic is that the oil droplet static contact angle at the surface of solids is more than 150 °.But, the surface tension of oil droplet is much smaller than the table of water droplet
Surface tension, therefore, preparation has the surface of solids of superoleophobic characteristic, and its difficulty is bigger than super hydrophobic surface, it more difficult to realize.Phase
Pass research shows, in air to be prepared, superoleophobic surface is in addition to needing the modification of low-surface-energy molecule, also will be at its band micro-nano
Rice introduces concave surface curvature on coarse structure surface so that micro-nano coarse structure is indent or cantilever-shaped.This gives and manufactures work
Skill proposes bigger challenge.
At present, substantial amounts of document is it has been reported that artificial bionic super hydrophobic surface, and these materials are at self-cleaning surface, anti-
Ice, antifog, anti-pollution, anticorrosion, fluid drag-reduction is widely used.Report about oleophobic surface is relatively fewer, but super
Oleophobic surface is such as grease proofness coating in industrial and agricultural production, the antifouling process of sea water, and petroleum pipeline is grease proofing creeps, in oil-water separation
There is huge application space.Metal material is widely applied in engineering, uses face extremely extensive, but the antipollution of metal is prevented
Corrosive nature is poor, and therefore on metal, preparation has superoleophobic characteristic surface and is significant.
So-called surface texture (Surface texture) refers to that body surface has certain size and the pit of arrangement, recessed
The array of the pattern such as trace or convex closure.Have the surface of micro-nano-scale microcosmic texture surface energy, optical characteristics, bionical characteristic,
The aspects such as mechanical property, hydrodynamic characteristics and friction and wear behavior and smooth surface show distinct feature, this
It is filled with new vitality for numerous disciplinary study, and shows huge application potential at many engineering fields.
The preparation method of oleophobic surface is generally followed from bottom to top or top-to-bottom method.Existing prepare superoleophobic surface
Process substantially have following several: (1) without template wet etching (2) femtosecond laser etching method (3) method of electrostatic spinning (4) electricity
Sedimentation (5) sol-gel process etc..
Prior art is primarily present following shortcoming: (1) can etch silicon and polymer surfaces, efficiency without template wet etching
High cost is low, but etching surface morphology controllable is poor, and this method is readily obtained super hydrophobic surface, but is difficult to obtain superoleophobic surface.
Oleophobic surface can be obtained by Bosch etching method, but complex process, with high costs；(2) femtosecond laser etching method can be prepared
Precision is high, the micro-nano nested structure surface of pattern rule, but this process efficiency is low, is not suitable for manufacturing on a large scale, and equipment is extremely
Expensive；(3) method of electrostatic spinning is by utilizing micro-/ nano filament at surface construction coarse structure, large area can prepare super-hydrophobic material
Material, but the controllability of the super hydrophobic material surface micro-structure prepared and uniformity are poor, wear no resistance, and service life is relatively
Short；(4) common electrodeposition process can deposit metal or polymer, can prepare the most easily and have micro-nano coarse structure table
Face, but pattern randomness is strong, wayward, and it is not likely to produce the secondary groove structure of indent or cantilever.
Summary of the invention
For the shortcoming of above-mentioned prior art, it is an object of the invention to propose one and utilize hot compression deformation method to prepare metal
The technique of the superoleophobic compound cast layer of base, is the improvement of conventional electrodeposition method, can produce the indent of morphology controllable or the two of cantilever
Secondary groove structure.
According to an aspect of the present invention, propose a kind of to utilize hot compression deformation method to prepare the superoleophobic compound cast layer of Metal Substrate
Method, comprises the steps: that the metallic substrates through deoiling is connected electricity as electroforming negative electrode, nickel plate as anode by (1)
Source, pass between the anode and cathode Dispersed precipitate have polymeric material microparticle ball Ni-based electroforming solution constitute electroforming system
System, energising make in electroforming solution polymer micropellet ball and nickel ion metal substrate surface codeposition formed thickness be about 50～
The Ni-based disperse composite electroforming deposit of 80um；(2) metallic substrates that deposition has after electro-deposition completes electroformed layer is carried out as anode
Electrolysis, removes one layer of nickel metal very thin on electroformed layer surface so that the polymer micropellet ball of the Dispersed precipitate revealed
Self is as micro-bulge structure；(3) height of surface of the work micro-bulge is ground by the workpiece precision grinder through Electrolyzed Processing
To basically identical；(4) a smooth straight pressing plate is warming up near the fusing point of selected polymeric material, keeps this temperature and incite somebody to action
It is positioned on the surface of the work micro-bulge prepared, and makes micro-bulge that non-homogeneous change occurs by the way of applying certain pressure
Shape, after deformation, the position near high temperature clamp surface broadens, and other positions only occur the least change, obtains opening less than interior
The superoleophobic concave inward structure in surface in chamber；(5) finally the carrying tablet of silicon fluoride is had to be collectively disposed in hermetic container with dripping workpiece
Row baking makes silicon fluoride pass through adsorption and forms the low-surface energy substance of one layer of nano thin-layer at surface of the work, finally makes metal
Surface reaches superoleophobic performance.
According to an aspect of the present invention, the material of microparticle ball is that thermoplastic polymer is (such as Low Density Polyethylene, PMMA
Deng), pressurizing and deformation of being heated, cooling and shaping.
According to an aspect of the present invention, the selection of microparticle ball must be consistent with particle diameter (20～30um), and it is at electroformed layer
Middle volume fraction controls in the range of 40～60%, and the spacing that the too small meeting of volume fraction makes particle sphere be distributed is excessive, volume fraction
Cross conference and affect the formation of cast layer.Particle diameter and the volume fraction of appropriate mix are so that forming opening less than inner chamber in subsequent handling
The superoleophobic concave inward structure in surface.
According to an aspect of the present invention, micro-bulge surface produces non-homogeneous thermal deformation, the most micro-when thermoplastic
When convex body surface flat surface smooth with high temperature contacts, it is higher that the thermoplastic near the position on high temperature surface is in temperature
State, its mobility and morphotropism are preferable, and the thermoplastic polymer temperature away from the position on high temperature surface is relatively low, mobility and
Morphotropism is poor, therefore can extrusion forming opening less than the superoleophobic concave inward structure in surface of inner chamber.
According to an aspect of the present invention, in step (2), electroforming solution adds appropriate surfactant, it
Can adsorb in large quantities micro-nano particle ball surface formed one layer of firm adsorbed film.
According to an aspect of the present invention, the micro-bulge extrusion forming opening of step (5) is superoleophobic less than the surface of inner chamber
Concave inward structure.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention；
Fig. 2 is the superoleophobic concave inward structure figure of the present invention.
Detailed description of the invention
Embodiments of the invention are described below in detail, and the example of described embodiment is shown in the drawings, the most from start to finish
Same or like label represents the element of same or like function.The embodiment described below with reference to accompanying drawing is to show
Example, it is only used for explaining the present invention, and is not considered as limiting the invention.On the contrary, embodiments of the invention include falling
Enter all changes, amendment and the equivalent in the range of the spirit of attached claims and intension.
Such as Fig. 1, a kind of method flow utilizing hot compression deformation method to prepare the superoleophobic compound cast layer of Metal Substrate is as follows:
S1, the pre-treatment of metallic substrates 1: after metallic substrates 1 is soaked oil removing with hot alkaline solution, with acetone and deionized water
Rinse further, be placed at 120 DEG C of vacuum drying oven dehydration 15min, to go the removal of impurity to make texture be connected jail with metallic substrates 1
Gu.
S2, metallic substrates 1 surface dispersion are composite electroformed: use nickel plate 2 as anode, metallic substrates 1 as negative electrode, both
Being connected respectively to positive pole and the negative pole of power supply 5, passing to Dispersed precipitate between the anode and cathode has the microparticle of polymeric material
The Ni-based electroforming solution 4 of ball 3, thus constitute electroforming system.Negative electrode generation reduction reaction after energising, makes polymer in electroforming solution 4 micro-
Granule ball 3 and nickel ion form, at metallic substrates 1 surface codeposition, the Ni-based disperse composite electroforming deposit that thickness is about 50～80um
6；
In this step, electrical quantity: electric current density 0.5～5A/dm2Square-wave pulse, frequency 0.5～3KHz, dutycycle
20～80%, process time (depending on cast layer thickness) etc.；Formulation of electroforming solution: Ni (CH2SO3)2·4H2O 200～500g/L,
NiCl2·6H2O 15～30g/L, H3BO330～45g/L, pH value about 4, temperature about 50 DEG C etc..
S3, the electrolysis of Ni-based disperse composite electroforming deposit: electro-deposition complete after by the anode and cathode reversal connection of electroforming system, make deposition
The metallic substrates 1 having electroformed layer 6 is electrolysed as anode.Anode generation oxidation reaction after energising, removes on electroformed layer 6 surface
One layer of very thin nickel metal so that the polymer micropellet ball 3 of the Dispersed precipitate revealed self is as micro-bulge 7.
In this step, by controlling electrical quantity: electric current density 10～15A/dm2Unidirectional current, process time (according to remove
Thickness is fixed) control the removal thickness (about particle sphere radius size) of nickel metal layer.Removal thickness is crossed conference and is caused particle sphere easy
Come off in cast layer, remove thickness too small, be not easily formed the needed micro-bulge of subsequent handling 7.
S4, polish micro-bulge: cleaned up by the workpiece taking-up deionized water through Electrolyzed Processing, will with precision grinder
The height of surface of the work micro-bulge 7 is milled to basically identical, then cleans up with deionized water and dry up with nitrogen.
S5, hot compression deformation: be warming up near the fusing point of selected polymeric material by a smooth straight pressing plate 8, keeping should
On the surface of the work micro-bulge 7 that temperature being placed on prepares, by between micro-bulge 7 surface and high temperature pressing plate 8 surface
The mode applying pressure (10Pa < P < 5000Pa) makes micro-bulge 7 that heterogeneous deformation to occur, near high temperature pressing plate 8 surface after deformation
Position broaden, and only there is the least change in other positions.Keep pressure and temperature certain time (after pressurization 5～10s), so
After high temperature pressing plate 8 is separated, be cooled to room temperature with the rate of temperature fall of 2～5 DEG C/min, after hot pressing obtained by micro-nano structure be
Opening is less than the superoleophobic concave inward structure in surface 9 of inner chamber.
S6, low-surface-energy are modified: by through the workpiece of Electrolyzed Processing with drip that to have the carrying tablet of silicon fluoride 10 to be collectively disposed at close
Close in container, be then placed in 65 DEG C of baking ovens and toast 1 hour, put after taking-up to room temperature, complete the preparation of workpiece.In baking process
In, silicon fluoride 10, by being formed the low-surface energy substance of one layer of nano thin-layer at surface of the work by adsorption, makes metal surface
Reach superoleophobic performance.
The workpiece finally prepared is as shown in Figure 2.
More preferably, in step sl, can be clear with the ultrasound wave filling ethanol solution to the metallic substrates 1 that surfacing is smooth
Washing machine is carried out, and recycles removal of surfactant oxidation on metal surface layer, finally cleans with deionized water and be placed in baking oven
Middle drying removes surface moisture.Make metallic substrates 1 surface cleaning clean free from admixture non-oxidation layer, it is simple to deposit on its surface
Metal level and metallic substrates have stronger adhesion.
More preferably, in step s 2, adding appropriate surfactant in electroforming solution, they can adsorb in large quantities
Micro-nano particle ball surface forms one layer of firm adsorbed film, can effectively prevent micro-nano particle from reuniting and being aided with super in electroforming system
Acoustic or electrical magnetic vibration is stirred, and more can promote particle suspension effect than simple mechanical type stirring.
Compared with prior art, advantages of the present invention has: 1) use the compound electric foundry work under suitable pulse electrical quantity
Skill is more easy to obtain fine and close smooth compound cast layer；2) can by select different polymer size, control hot plate temperature and
Pressurization size obtains the structure of different concave curvature, thus obtains the surface of the work that oleophobic property is controlled；3) skill that this invention uses
Art and equipment are simple, with low cost, it is adaptable to the superoleophobic modification in large-area metal surface.
In the case of spiritual without departing from the present invention or necessary characteristic, the present invention can be embodied in other specific forms.Should
Described specific embodiment each side is considered merely as illustrative and non-limiting.Therefore, scope of the invention such as appended claims
Scope is shown rather than shown as indicated above.All fall change in the equivalent meaning and scope of claim should be regarded as
Fall in the category of claim.
Claims (7)
1. the method utilizing hot compression deformation method to prepare the superoleophobic compound cast layer of Metal Substrate, comprises the steps: that (1) will be passed through
The metallic substrates of deoiling connects power supply as electroforming negative electrode, nickel plate as anode, passes to disperse between the anode and cathode
The Ni-based electroforming solution of the microparticle ball that polymeric material is distributed constitutes electroforming system, and energising makes polymer micropellet in electroforming solution
Ball and nickel ion form, at metal substrate surface codeposition, the Ni-based disperse composite electroforming deposit that thickness is about 50～80um；(2) electricity
The metallic substrates that deposition has after having deposited electroformed layer is electrolysed as anode, removes very thin on electroformed layer surface one layer
Nickel metal so that the polymer micropellet ball of the Dispersed precipitate revealed self is as micro-bulge structure；(3) will be through electrolysis
The height of surface of the work micro-bulge is milled to basically identical by the workpiece precision grinder of processing；(4) by a smooth straight pressing plate
It is warming up near the fusing point of selected polymeric material, keeps this temperature and be placed on the surface of the work micro-bulge prepared
On, by the way of applying certain pressure, make micro-bulge generation heterogeneous deformation, near the position of high temperature clamp surface after deformation
Broaden, and other positions only occur the least change, obtain the opening superoleophobic concave inward structure in surface less than inner chamber；(5) last
By workpiece with drip and have the carrying tablet of silicon fluoride to be collectively disposed in hermetic container to carry out baking and make silicon fluoride pass through adsorption in work
Part surface forms the low-surface energy substance of one layer of nano thin-layer, finally makes metal surface reach superoleophobic performance.
Utilizing the method that hot compression deformation method prepares the superoleophobic compound cast layer of Metal Substrate the most as claimed in claim 1, its feature exists
In, the material of described polymer micropellet ball is thermoplastic polymer.
Utilizing the method that hot compression deformation method prepares the superoleophobic compound cast layer of Metal Substrate the most as claimed in claim 1, its feature exists
In, the material of described polymer micropellet ball is Low Density Polyethylene or PMMA.
Utilizing the method that hot compression deformation method prepares the superoleophobic compound cast layer of Metal Substrate the most as claimed in claim 1, its feature exists
In, the selection of described polymer micropellet ball must be consistent with particle diameter, and its size is 20～30um, and it is volume in electroformed layer
Fractional domination is in the range of 40～60%.
Utilizing the method that hot compression deformation method prepares the superoleophobic compound cast layer of Metal Substrate the most as claimed in claim 1, its feature exists
In, in step (1), the metallic substrates smooth to surfacing can be carried out clearly with the ultrasonic washing unit filling ethanol solution
Wash, recycle removal of surfactant oxidation on metal surface layer, finally clean with deionized water to be placed in baking oven drying and remove
Surface moisture.
Utilizing the method that hot compression deformation method prepares the superoleophobic compound cast layer of Metal Substrate the most as claimed in claim 1, its feature exists
In, in step (2), electroforming solution adding appropriate surfactant, they can adsorb in large quantities at micro-nano particle ball
Surface forms one layer of firm adsorbed film.
Utilizing the method that hot compression deformation method prepares the superoleophobic compound cast layer of Metal Substrate the most as claimed in claim 1, its feature exists
In, the micro-bulge extrusion forming opening of step (5) is less than the superoleophobic concave inward structure in surface of inner chamber.
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| CN201610534243.2A CN106048665B (en) | 2016-07-07 | 2016-07-07 | A kind of method that the superoleophobic compound cast layer of Metal Substrate is prepared using hot compression deformation method |
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Cited By (2)
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| CN106906469A (en) * | 2017-04-25 | 2017-06-30 | 广东工业大学 | A kind of micro-nano nesting particle fusion self-bonding surface modifying apparatus |
| WO2018196346A1 (en) * | 2017-04-25 | 2018-11-01 | 广东工业大学 | Metal surface modification apparatus |
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| WO2018196346A1 (en) * | 2017-04-25 | 2018-11-01 | 广东工业大学 | Metal surface modification apparatus |
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