CN117265528B - Wear-resistant super-wetting surface and preparation method thereof - Google Patents
Wear-resistant super-wetting surface and preparation method thereof Download PDFInfo
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- 239000002923 metal particle Substances 0.000 claims description 25
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- 238000001816 cooling Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- XPBBUZJBQWWFFJ-UHFFFAOYSA-N fluorosilane Chemical compound [SiH3]F XPBBUZJBQWWFFJ-UHFFFAOYSA-N 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 244000025254 Cannabis sativa Species 0.000 claims description 7
- 239000003570 air Substances 0.000 claims description 7
- 239000010953 base metal Substances 0.000 claims description 7
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- 239000003607 modifier Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005054 agglomeration Methods 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
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- 239000011651 chromium Substances 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 3
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- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
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- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 229920000548 poly(silane) polymer Polymers 0.000 claims description 3
- 229920002620 polyvinyl fluoride Polymers 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
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- 229910052725 zinc Inorganic materials 0.000 claims description 3
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
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Classifications
-
- 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
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The invention belongs to the technical field of super-wetting film synthesis, and particularly relates to a wear-resistant super-wetting surface and a preparation method thereof. The method comprises the following steps: and cleaning the metal piece, and then irradiating the surface of the metal piece with pulse laser according to a required pattern to form micro-nano rough metal, grass-shaped aggregated metal oxide and cauliflower-shaped aggregated metal oxide in a second area, so as to obtain the metal piece with the wear-resistant super-wetting surface. According to the preparation method of the wear-resistant super-wetting surface, the shape and the track of laser irradiation are designed, the irradiated part forms a micro-nano rough area containing metal oxide, the non-irradiated part can form a frame structure connected with each other, the wear-resistant effect is provided, and the rough super-wetting structure and the wear-resistant structure are formed in one step through a simple process of laser irradiation.
Description
Technical Field
The invention belongs to the technical field of super-wetting film synthesis, and particularly relates to a wear-resistant super-wetting surface and a preparation method thereof.
Background
The super-wetting film layer comprises a super-hydrophilic film layer and a super-hydrophobic film layer, the water contact angle of the super-hydrophilic film layer is close to 0 degrees, and the super-wetting film layer is strongly hydrophilic, so that the super-wetting film layer can be applied to the fields of liquid transmission, catalysis and the like; the contact angle of the super-hydrophobic material with water is larger than 150 degrees, water drops, rainwater and the like can flow away rapidly when falling on the surface and keep the surface clean, and the super-hydrophobic material has wide application prospects in the fields of anti-icing, self-cleaning, oil-water separation, corrosion resistance, antibacterial and the like. The super-moist film layer on the metal surface has been studied in a large quantity, but the film layer has the problems of poor wear resistance and poor bonding force with a substrate, and the film layer is damaged and falls off due to contact with a hard object, so that the performance is reduced. In order to improve the abrasion resistance of superhydrophobic films, there have been many studies, such as by using an adhesive to bond between the coating and the substrate, introducing a random discrete microstructure to perform abrasion resistance, or by sacrificing the film itself or a roughened columnar structure in the film to achieve the effect of improving abrasion resistance. The existing laser etching structure metal surface super-wetting film layer takes laser etching as a 'nicking tool' for constructing arrays such as cylinders, cones and the like, removes metal on the surface, forms various micro-or nano-structures, and forms micro-nano structures required by the super-hydrophobic film layer. The corrosion resistance of the super-wetting film layer is improved to a certain extent by the exploration, but the improvement degree is limited, the process is complex, and the practicability is required to be improved.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a wear-resistant super-wetting surface and a preparation method thereof. The abrasion-resistant super-wetting surface is a laser oxidation abrasion-resistant super-wetting surface.
The object of the invention is achieved by at least one of the following technical solutions.
The method provided by the invention is a method for oxidizing the super-wetted surface by laser; the method controls the rough surface formed by laser irradiation oxidation and the unirradiated frame structure by controlling the laser irradiation track and the laser parameters, thereby forming the rough structure and the wear-resistant frame structure in one step, presenting super-hydrophilic performance, and forming the wear-resistant super-hydrophobic film layer after hydrophobic modification.
The laser oxidation wear-resistant super-wetting surface comprises a first area and a second area; the first region is a non-oxidation region, and the second region is an oxidation region; the thickness of the first area in the vertical direction of the laser oxidation abrasion-resistant super-wetting surface is not smaller than that of the second area; the second region includes micro-nano rough metal and metal oxide.
The first region divides the second region into an array or non-array region.
Further, the second area accounts for 25% -100% of the laser oxidation abrasion-resistant super-wetting surface area; the second areas are divided into regular and irregular arrangement, the number of the second areas is not less than 1, and the shape of each second area is one of square, rectangle, triangle, diamond, circle and hexagon.
Further, the metal oxide includes a first aggregated form and a second aggregated form, the first aggregated form of metal oxide being a grass-like aggregated metal oxide (first metal oxide); the second aggregated form of the metal oxide is a cauliflower-like aggregated metal oxide (second metal oxide).
The ratio of the metal oxides in the first and second aggregate forms is affected by the degree of oxidation, and the first oxide ratio is high when the degree of oxidation is low and the second oxide ratio is low when the degree of oxidation is high.
Further, the grass-like aggregated metal oxide has a degree of aggregation that is less than that of the cauliflower-like aggregated metal oxide; the thickness of the grass-shaped aggregated metal oxide in the vertical direction of the laser oxidation abrasion-resistant super-wetting surface is not larger than that of the cauliflower-shaped aggregated metal oxide. The metal oxide in the second aggregated form may be converted from the metal oxide in the first aggregated form.
Further, the grass-like aggregated metal oxide includes a metal particle surface oxide (third metal oxide) and a surface oxide (fourth metal oxide) of which the base molten metal is re-cooled and solidified; the thickness of the metal particle surface oxide in the vertical direction of the laser oxidation abrasion-resistant super-wetting surface is not smaller than the thickness of the surface oxide of the substrate molten metal which is cooled and solidified again.
The agglomeration degree of the surface oxide of the metal particles is not less than that of the surface oxide solidified by cooling the molten metal of the substrate.
The second region further comprises a micro-nano rough metal layer; the micro-nano rough metal layer comprises base metal, molten cooled metal and sputtered metal particles, and the metal oxide covers the surface of the metal layer;
the third metal oxide covers the surfaces of the metal particles, the fourth metal oxide covers the surfaces of the metal particles after being melted and cooled, and the second metal oxide in a gathered form covers the surfaces of part of the sputtered metal particles;
The number of the third metal oxides is denoted as N3, the number of the fourth metal oxides is denoted as N2, and the number of the second aggregated form of metal oxides is denoted as N1;
Then there is
1≤N1/N3≤50；
1≤N1/(N2+N3)≤50。
The invention provides a preparation method of an abrasion-resistant super-wetting surface, which comprises the following steps:
Cleaning a metal piece, then irradiating the surface of the metal piece with pulse laser according to a required pattern (the irradiation energy of the laser is higher and exceeds the threshold value of metal oxidation, and simultaneously, the laser is exploded to form sputtering metal particles for accumulation, molten metal is cooled and recast, concave-convex arrangement of matrix metal is overlapped to form a micro-nano coarse structure skeleton arranged in an array, part of metal forms metal oxide under the action of the laser and covers the surface of the skeleton to form a part of providing wettability on the target surface), and grass-shaped aggregated metal oxide and cauliflower-shaped aggregated metal oxide in a second area are formed to obtain the metal piece comprising the laser oxidation wear-resistant super-wetting surface.
Further, the metal is more than one of copper, silver, aluminum, titanium, magnesium, iron, zinc, chromium, nickel and alloys of the metals; the pulse laser is nanosecond pulse laser; the power of the pulse laser is more than 0.1W; the irradiation speed of the pulse laser irradiation is 0.1-1000mm/s, and the pulse frequency of the pulse laser is 1 kHz-100 kHz; the diameter of the beam spot of the laser beam of the pulse laser is 10-500 mu m, and the number of irradiation cycles of the pulse laser is 1-50 times;
Further, the atmosphere of the pulse laser when irradiation is performed is one or more of air, nitrogen, argon, helium and oxygen.
Further, the atmosphere at the time of irradiation with the pulse laser may provide a carbon source, a nitrogen source, and an argon source; coating silane or boron paste on the metal surface to provide a silicon source and a boron source; the metal surface can be covered with silicon dioxide, diamond, silicon carbide and the like, a physical wear-resistant phase can be provided, and the surface is strengthened after laser irradiation.
Further, the distance between the laser adjacent routes when the pulse laser irradiates the surface of the metal piece is not larger than the spot diameter, and the difference between the distance between the laser adjacent routes and the spot diameter when the pulse laser irradiates the surface of the metal piece is smaller than 50 μm. When the high-energy density laser irradiates the metal, rapid burst boiling occurs, the material is sputtered in the form of a mixture of molten liquid drops and high-temperature vapor, metal particles are formed in the cooling process, the molten metal is re-solidified, and meanwhile, the sputtered liquid vapor forms metal oxide to be attached to the rough metal surface in an oxidation environment and a high-temperature environment.
Further, the metal piece containing the laser oxidation abrasion-resistant super-wetting surface (the super-hydrophilic surface is formed after the metal surface is irradiated by pulse laser) is soaked in a modifier for low surface energy substance treatment, so that a super-hydrophobic surface is formed; the modifier is more than one of fluorosilane, stearic acid, siloxane polysilane and polyvinyl fluoride; the soaking time is 10min to 12h.
Further, after cleaning the metal piece, covering the surface of the metal piece with a wear-resistant phase material, and then carrying out pulse laser irradiation; the physical wear-resistant phase material is more than one of silicon dioxide, diamond and silicon carbide.
The pattern of the second area can be directly and completely printed by laser, or can be intermittently irradiated by a laser, and the metal moves at a certain speed to form an array pattern or a non-array pattern.
Compared with the prior art, the invention has the following advantages and beneficial effects:
The preparation method of the super-wetting surface comprises a chemical method, an electrochemical method, a template method and the like, and the surface tends to have poor wear resistance. The existing technology for improving the wear resistance of the super-wet film layer is provided with an etched columnar array to improve the wear resistance, or wear-resistant components are added into the film layer, the wear resistance of the technology can not meet the requirements, or the equipment and the technology are too complex to meet the actual requirements;
According to the preparation method of the laser oxidation super-wetting film layer, the shape and the track of laser irradiation are designed, the irradiated part forms a micro-nano rough area containing metal oxide, the non-irradiated part can form a frame structure connected with each other, the wear-resistant effect is provided, and the rough super-wetting structure and the wear-resistant structure are formed in one step through a simple process of laser irradiation. The preparation method of the laser oxidation super-wetting film layer provided by the invention can be used for preparing the wear-resistant super-wetting film layer meeting different requirements through laser fine processing; the preparation method of the laser oxidation super-wetting film layer provided by the invention forms a coarse structure and a frame structure by laser selective irradiation in one step, and has strong practicability. The super-wetting surface can be applied to the super-hydrophobic field and the super-hydrophilic field, and can also be applied to self-cleaning, corrosion resistance and pollution prevention. Anti-icing, oil-water separation, antibacterial, catalytic and other fields.
Drawings
FIG. 1 is an optically magnified photograph of the super-wetted surface of example 1; and marking the region above the laser oxidation abrasion-resistant super-wetting surface, and marking the region below the second region of the super-wetting surface.
Fig. 2 is a photograph of a profile of a laser oxidized abrasion resistant super-wetted surface of example 1, with square areas as the second areas and frame structures as the first areas.
FIG. 3 is a microstructure view of the laser oxidized abrasion resistant super-wetted surface of example 1.
Fig. 4 is a structural topography of the second region of the laser oxidized abrasion resistant super-wetted surface of example 1.
Fig. 5 is a structural topography of the second metal oxide laser oxidized super wetted surface of example 1.
Fig. 6 is a graph of the morphology of three oxide structures of example 1 laser oxidized super-wetted surfaces.
Fig. 7 is a structural morphology of the low power laser oxidized super-wetted surface of example 2.
FIG. 8 is a schematic diagram of a laser oxidation process performed in an example.
FIG. 9 is a schematic view of a first zone and a second zone structural arrangement; wherein the black region is a first region, the oxidized region, the white region is a second region, and the non-oxidized region.
FIG. 10 is a graph of the surface microtopography of example 3 using an infrared laser.
FIG. 11 is a chart showing the micro-morphology of the second region of the Ti metal surface in example 4.
FIG. 12 is a photograph of the hydrophobic angle of the laser oxidized surface in example 5.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but are not intended to limit the practice and protection of the invention. It should be noted that the following processes, if not specifically described in detail, can be realized or understood by those skilled in the art with reference to the prior art. The reagents or apparatus used were not manufacturer-specific and were considered conventional products commercially available.
Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings. In the following description, like modules are denoted by like reference numerals. In the case of the same reference numerals, their names and functions are also the same. Therefore, a detailed description thereof will not be repeated.
The abrasion-resistant super-wetting surface provided by the embodiment of the invention is divided into a first area (a non-oxidation area) and a second area (an oxidation area); the first region is a non-oxidized region, and the second region is an oxidized region. Referring to FIG. 1, FIG. 1 is an optically magnified photograph of the super-wetted surface of example 1; the upper part of the figure is marked as a mixed region of the first region and the second region of the laser-oxidized abrasion-resistant super-wetted surface, and the lower part of the figure is marked as the second region of the super-wetted surface.
Referring to fig. 2, fig. 2 is a profile photograph of a laser oxidation abrasion-resistant super-wetting surface according to example 1, wherein a square region is the second region, a frame structure is the first region, and the height of the first region in the Z direction is greater than or equal to the height of the second region in the Z direction (the thickness of the first region in the perpendicular direction of the laser oxidation abrasion-resistant super-wetting surface is not smaller than the second region);
The first region divides the second region into array regions (see fig. 1 and 3); the first region has an abrasion-resistant effect, the second region has a super-wetting effect, when the super-wetting surface is rubbed, the super-wetting surface preferentially acts on the first region,
The second region is substantially unaffected and the super-wetting effect is still present.
The second region comprises two (aggregate) forms of metal oxide: the first metal oxide aggregates in a grass shape and the second metal oxide aggregates in a cauliflower shape (see fig. 4 and 5).
The average height of the first metal oxide (the first aggregate form metal oxide) in the Z-axis direction is less than or equal to the average height of the second metal oxide (the second aggregate form metal oxide) in the Z-axis direction (namely, the thickness of the grass-like aggregate metal oxide in the vertical direction of the laser oxidation abrasion-resistant super-wetting surface is not greater than that of the cauliflower-like aggregate metal oxide, see fig. 4 and 6);
The ratio of the first oxide to the second oxide is affected by the degree of oxidation, and the first oxide is high in proportion to the low degree of oxidation and the second oxide is low in proportion to the high degree of oxidation.
The first oxide has a degree of agglomeration smaller than that of the second metal oxide (metal oxide in the second aggregated form); the second oxide may be converted from the first oxide.
The first metal oxide (first aggregate form of metal oxide) comprises two different oxides, a third metal oxide (metal particle surface oxide), a fourth metal oxide (base molten metal re-cooled solidified surface oxide), see fig. 6.
Wherein the average height of the third metal oxide in the Z-axis direction is not less than or equal to the average height of the fourth metal oxide in the Z-axis direction (the thickness of the surface oxide of the metal particles in the vertical direction of the laser oxidation abrasion-resistant super-wetting surface is not less than the thickness of the surface oxide of the substrate molten metal which is cooled and solidified again); the third oxide is agglomerated to a degree not less than that of the fourth metal oxide.
The second region further comprises a micro-nano rough metal layer, wherein the metal layer comprises: the metal oxide covers the surface of the metal layer;
The third metal oxide covers the surface of the metal particles, the fourth metal oxide covers the surface of the metal after being melted and cooled, and the second metal oxide covers the surface of part of the sputtered metal particles (figure 6);
The number of the third metal oxides (metal particle surfaces) was designated as N3, the number of the fourth metal oxides (molten metal recooling solidification surfaces) was designated as N2, and the number of the second aggregated form of the metal oxides was designated as N1;
Then there is
1≤N1/N3≤50；
1≤N1/(N2+N3)≤50。
The array second region shape includes: square, rectangular, triangular, diamond, circular, and hexagonal (see fig. 9), the second region comprising from 25% to 100% of the total area; the second area occupies less than 25 percent of the area, so that the super-wetting effect cannot be achieved, and the wear-resisting effect is the worst when the area occupied is 100 percent; ) The first area has an abrasion-resistant effect, the second area has a super-wetting effect, the second area is not higher than the first area, when the super-wetting surface is rubbed, the super-wetting surface preferentially acts on the first area, the second area is not affected basically, and the super-wetting effect still exists.
Referring to fig. 8, a method for preparing an abrasion-resistant laser oxidized super-wetted surface comprises the following steps:
s1, cleaning a metal piece;
S2, according to laser parameters and designed array patterns, pulse laser irradiates the surface of a metal piece, irradiation energy of the laser is higher and exceeds a metal oxidation threshold value, phase explosion occurs simultaneously, sputtered metal particles are formed to be stacked, molten metal is cooled and recast, concave-convex arrangement of matrix metal is overlapped, a micro-nano coarse structure framework of array arrangement is formed, metal oxide covers the surface of the framework, and a part of a target surface providing wettability is formed.
The preparation method S1 of the laser oxidation super-wetting film layer, wherein the metal is one or more of copper, silver, aluminum, titanium, magnesium, iron, zinc, chromium, nickel and alloys thereof.
The preparation method S2 of the laser oxidation super-wetting film layer is characterized in that the power of the nanosecond pulse laser is larger than 0.1W, the irradiation rate of the nanosecond pulse laser is 0.1-1000mm/S, the pulse frequency is 1 kHz-100 kHz, the beam spot diameter of the laser beam is 5-500 mu m, the number of irradiation cycles is 1-100, and the laser parameters can be different in non-single cycle. The atmosphere of the nanosecond pulse laser is one or more of air, nitrogen, argon, helium and oxygen when the nanosecond pulse laser irradiates.
In the preparation method S2 of the laser oxidation super-wetting film layer, when the laser irradiates on the metal surface, the distance between the adjacent routes of the laser is smaller than the diameter of a light spot and smaller than 500 mu m. The difference between the distance between the adjacent routes of the laser and the diameter of the light spot is less than 50 mu m.
The preparation method S2 of the laser oxidation super-moist film layer comprises the following steps of: when the high-energy density laser irradiates the metal, rapid burst boiling occurs, the material is sputtered in the form of a mixture of molten liquid drops and high-temperature vapor, metal particles are formed in the cooling process, the molten metal is re-solidified, and meanwhile, the sputtered liquid vapor forms metal oxide to be attached to the rough metal surface in an oxidation environment and a high-temperature environment.
The preparation method S2 of the laser oxidation super-wetting film layer can directly form an array pattern, or can intermittently irradiate a laser, and metal moves at a certain speed to form the array pattern.
The preparation method S3 of the laser oxidation super-wetting film layer is characterized in that after the metal surface is irradiated by nanosecond pulse laser, a super-hydrophilic surface is formed, and the metal surface is subjected to low surface energy material treatment to form a super-hydrophobic surface; the low surface energy material treatment includes: immersing the metal irradiated by the pulse laser in a modifier; the modifier is more than one of fluorosilane, stearic acid, siloxane polysilane and polyvinyl fluoride; the soaking time is 10min to 12h.
The atmosphere of the laser oxidation super-wetting film layer can provide a carbon source, a nitrogen source and an argon source; coating silane or boron paste on the metal surface to provide a silicon source and a boron source; the metal surface can be covered with silicon dioxide, diamond, silicon carbide and the like, a physical wear-resistant phase can be provided, and the surface is strengthened after laser irradiation.
Example 1
The preparation method of the laser oxidation super-wetting surface provided in the embodiment 1 comprises the following steps:
s1, carrying out acid washing, water washing, oil removal, ultrasonic cleaning in deionized water and the like on a copper plate;
s2, processing the surface of the copper plate by ultraviolet laser to obtain an array pattern;
S2-1, processing the surface of the copper plate by adopting ultraviolet lasers with different parameters according to requirements, determining the selected laser parameters, wherein the diameter of a light spot is 10 mu m, the laser irradiation speed is 10mm/S, the frequency is 20Khz, the laser irradiation times are 1 time, and the power of ultraviolet laser processing is in the range of 1.5-5W;
s2-2, then preparing a second area, wherein the distance between the adjacent parallel lines of the laser is 30 mu m, and the adjacent parallel lines of the laser are used for forming the micro-nano structure, the width of the frame in the first area is 50 mu m, and the atmosphere is air.
S2-3, adopting preset ultraviolet laser parameters and a second area pattern, and irradiating the surface of the copper plate by using a laser until the laser processing is finished. At this point, an abrasion-resistant super-wetted surface is formed;
And S3, soaking the metal subjected to ultraviolet laser processing in an alcoholic solution of fluorosilane for 1h, and then drying in a drying oven at 100 ℃ for 1h to form an abrasion-resistant super-hydrophobic surface on the surface of the copper plate.
The wear-resistant super-hydrophobic surface comprises a first area and a second area, wherein the first area is a non-oxidation area, the second area is an oxidation area, the first area divides the second area into an array shape, and the thickness of the second area in the vertical direction of the laser oxidation wear-resistant super-wetting surface is 100 mu m. The second region area accounts for 90% of the laser-oxidized abrasion-resistant super-wetting surface area (the shape of a single second region is square). The second region comprises a micro-nano rough metal layer; the micro-nano rough metal layer comprises base metal, metal after melting and cooling and sputtered metal particles, and the metal oxide covers the surface of the micro-nano rough metal layer; the metal oxide comprises a first aggregation form and a second aggregation form, wherein the first aggregation form is a grass aggregation metal oxide; the metal oxide in the second aggregation form is a cauliflower-shaped aggregation metal oxide.
The super-wetted surface was tested with a contact angle meter, the drop was 5 microliters deionized water, the contact angle of the water was measured, the drop contact angle was less than 30 ° before modification (i.e., the copper plate of S1), and 158 ° after modification (i.e., the abrasion-resistant super-hydrophobic surface of S3), as shown in fig. 12.
The super-wetted surface of the copper plate was rubbed repeatedly using 400 mesh sandpaper, and then a drop of 5 μl deionized water was dropped onto the copper laser machined surface, and the drop contact angle was measured to be 154 °.
Example 2
The preparation method of the laser oxidation super-wetting surface provided in the embodiment 2 comprises the following steps:
s1, carrying out acid washing, water washing, oil removal, ultrasonic cleaning in deionized water and the like on a copper plate;
s2, processing the surface of the copper plate by ultraviolet laser to obtain an array pattern;
s2-1, processing the surface of the copper plate by adopting ultraviolet lasers with different parameters according to requirements, determining the selected laser parameters, wherein the diameter of a light spot is 10 mu m, the laser irradiation speed is 10mm/S, the frequency is 15Khz, the laser irradiation times are 1 time, and the power of ultraviolet laser processing is in the range of 0.5-1W;
s2-2, then designing a second area, wherein the distance between the adjacent parallel lines of the laser is 30 mu m, and the adjacent parallel lines of the laser are used for forming the micro-nano structure, the width of the frame in the first area is 30 mu m, and the atmosphere is air.
S2-3, adopting preset ultraviolet laser parameters and a second area pattern, and irradiating the surface of the copper plate by using a laser until the laser processing is finished. At this point an abrasion resistant super-wetted surface is formed (see fig. 7); the first metal oxide comprises about 5% of the surface oxide.
And S3, soaking the metal subjected to ultraviolet laser processing in an alcoholic solution of fluorosilane for 1h, and then drying in a drying oven at 100 ℃ for 1h to form an abrasion-resistant super-hydrophobic surface on the surface of the copper plate.
The wear-resistant super-hydrophobic surface comprises a first area and a second area, wherein the first area is a non-oxidation area, the second area is an oxidation area, the first area divides the second area into an array pattern, and the thickness of the second area in the vertical direction of the laser oxidation wear-resistant super-wetting surface is 20 mu m. The second area occupies 90% of the laser oxidized abrasion resistant super wetting surface area; the shape of the single second region is square. The second region comprises a micro-nano rough metal layer; the micro-nano rough metal layer comprises base metal, metal after melting and cooling and sputtered metal particles, and the metal oxide covers the surface of the micro-nano rough metal layer; the metal oxide comprises a first aggregation form and a second aggregation form, wherein the first aggregation form is a grass aggregation metal oxide; the metal oxide in the second aggregation form is a cauliflower-shaped aggregation metal oxide.
The super-wetted surface was tested with a contact angle meter, the drop was 5 microliters deionized water, the contact angle of the water was measured, the drop contact angle was less than 30 ° before modification (i.e., the copper plate of S1), and 150 ° after modification (i.e., the abrasion-resistant super-hydrophobic surface of S3), as shown in fig. 12.
The super-wetted surface of the copper plate was rubbed repeatedly using 400 mesh sandpaper, and then a drop of 5 μl deionized water was dropped onto the copper laser machined surface, measuring the drop contact angle as 148 °.
Example 3
The preparation method of the laser oxidation super-wetting surface provided in the embodiment 3 comprises the following steps:
s1, carrying out acid washing, water washing, oil removal, ultrasonic cleaning in deionized water and the like on a copper plate;
s2, processing the surface of the copper plate by using infrared laser to obtain an array pattern;
S2-1, processing the surface of the copper plate by adopting infrared lasers with different parameters according to requirements, determining the selected laser parameters, wherein the diameter of a light spot is 10 mu m, the laser irradiation speed is 5mm/S, the frequency is 20Khz, the laser irradiation times are 1 time, and the power of infrared laser processing is in the range of 40-50W;
S2-2, designing a second area, wherein the distance between adjacent parallel laser routes is 30 mu m, the adjacent parallel laser routes are used for forming micro-nano structures, the width of a frame in the first area is 50 mu m, and the atmosphere is air;
S2-3, adopting preset infrared laser parameters and a second area pattern, and irradiating the surface of the copper plate by using a laser until the laser processing is finished. At this point an abrasion resistant super-wetted surface is formed (see fig. 10);
And S3, soaking the metal subjected to infrared laser processing in an alcoholic solution of fluorosilane for 1h, and then drying in a drying oven at 100 ℃ for 1h to form an abrasion-resistant superhydrophobic surface on the surface of the copper plate.
The wear-resistant super-hydrophobic surface comprises a first area and a second area, wherein the first area is a non-oxidation area, the second area is an oxidation area, the first area divides the second area into an array pattern, and the thickness of the second area in the vertical direction of the laser oxidation wear-resistant super-wetting surface is 60 mu m. The second area occupies 90% of the laser oxidized abrasion resistant super wetting surface area; the shape of the single second region is square. The second region comprises a micro-nano rough metal layer; the micro-nano rough metal layer comprises base metal, metal after melting and cooling and sputtered metal particles, and the metal oxide covers the surface of the micro-nano rough metal layer; the metal oxide comprises a first aggregation form and a second aggregation form, wherein the first aggregation form is a grass aggregation metal oxide; the metal oxide in the second aggregation form is a cauliflower-shaped aggregation metal oxide.
The super-wetted surface was tested with a contact angle meter, the drop was 5 microliters deionized water, the contact angle of the water was measured, the drop contact angle was less than 30 ° before modification (i.e. the copper plate of S1), 153 ° after modification (i.e. the abrasion resistant super-hydrophobic surface of S3), and reference was made to fig. 12.
The super-wetted surface of the copper plate was rubbed repeatedly using 400 mesh sandpaper, and then a drop of 5 microliters deionized water was dropped onto the copper laser machined surface, measuring a drop contact angle of 149 °.
Example 4
S1, carrying out acid washing, water washing, oil removal, ultrasonic cleaning in deionized water and the like on a titanium plate;
s2, processing the surface of the titanium plate by ultraviolet laser to obtain an array pattern;
S2-1, processing the surface of the titanium plate by adopting ultraviolet lasers with different parameters according to requirements, determining the selected laser parameters, wherein the spot diameter is 10 mu m, the laser irradiation speed is 10mm/S, the frequency is 20Khz, the laser irradiation times are 1 time, and the power of ultraviolet laser processing is in the range of 1.5-5W;
S2-2, then designing a second area, wherein the distance between the adjacent parallel lines of the laser is 30 mu m, and the adjacent parallel lines of the laser are used for forming the micro-nano structure, the width of the frame in the first area is 50 mu m, and the atmosphere is air.
S2-3, irradiating the surface of the titanium plate by using a laser with preset ultraviolet laser parameters and a second area pattern until the laser processing is finished. At this point an abrasion resistant super-wetted surface is formed (see fig. 11);
S3, soaking the metal subjected to ultraviolet laser processing in an alcoholic solution of fluorosilane for 1h, and then drying in a drying oven at 100 ℃ for 1h to form an abrasion-resistant superhydrophobic surface on the surface of the titanium plate.
The wear-resistant super-hydrophobic surface comprises a first area and a second area, wherein the first area is a non-oxidation area, the second area is an oxidation area, the first area divides the second area into an array pattern, and the thickness of the second area in the vertical direction of the laser oxidation wear-resistant super-wetting surface is 100 mu m. The second area occupies 90% of the laser oxidized abrasion resistant super wetting surface area; the shape of the single second region is square. The second region comprises a micro-nano rough metal layer; the micro-nano rough metal layer comprises base metal, metal after melting and cooling and sputtered metal particles, and the metal oxide covers the surface of the micro-nano rough metal layer; the metal oxide comprises a first aggregation form and a second aggregation form, wherein the first aggregation form is a grass aggregation metal oxide; the metal oxide in the second aggregation form is a cauliflower-shaped aggregation metal oxide.
The super-wetted surface was tested with a contact angle meter, the drop was 5 microliters deionized water, the contact angle of the water was measured, the drop contact angle was less than 30 ° before modification (i.e., the titanium plate of S1), and 155 ° after modification (i.e., the abrasion-resistant super-hydrophobic surface of S3), as shown in fig. 12.
The super-wetted surface of the titanium plate was repeatedly rubbed using 400 mesh sandpaper, and then 5 μl of deionized water was dropped on the copper laser machined surface, and the drop contact angle was measured to be 152 °.
Example 5
S1, carrying out acid washing, water washing, oil removal, ultrasonic cleaning in deionized water and the like on a copper plate;
s2, processing the surface of the copper plate by ultraviolet laser to obtain an array pattern;
s2-1, processing the surface of the copper plate by adopting ultraviolet lasers with different parameters according to requirements, determining the selected laser parameters, wherein the diameter of a light spot is 50 mu m, the laser irradiation speed is 10mm/S, the frequency is 25Khz, the laser irradiation times are 1 time, and the power of ultraviolet laser processing is in the range of 3.5-5W;
S2-2, designing a second area, wherein the distance between adjacent parallel laser routes is 30 mu m, the adjacent parallel laser routes are used for forming micro-nano structures, the width of a frame in the first area is 50 mu m, and the atmosphere is oxygen atmosphere;
S2-3, adopting preset ultraviolet laser parameters and a second area pattern, and irradiating the surface of the copper plate by using a laser until the laser processing is finished. At this point, an abrasion-resistant super-wetted surface is formed;
And S3, soaking the metal subjected to ultraviolet laser processing in an alcoholic solution of fluorosilane for 1h, and then drying in a drying oven at 100 ℃ for 1h to form an abrasion-resistant super-hydrophobic surface on the surface of the copper plate.
The wear-resistant super-hydrophobic surface comprises a first area and a second area, wherein the first area is a non-oxidation area, the second area is an oxidation area, the first area divides the second area into an array pattern, and the thickness of the second area in the vertical direction of the laser oxidation wear-resistant super-wetting surface is 100 mu m. The second area occupies 90% of the laser oxidized abrasion resistant super wetting surface area; the shape of the single second region is square. The second region comprises a micro-nano rough metal layer; the micro-nano rough metal layer comprises base metal, metal after melting and cooling and sputtered metal particles, and the metal oxide covers the surface of the micro-nano rough metal layer; the metal oxide comprises a first aggregation form and a second aggregation form, wherein the first aggregation form is a grass aggregation metal oxide; the metal oxide in the second aggregation form is a cauliflower-shaped aggregation metal oxide.
The super-wetted surface was tested with a contact angle meter, the drop was 5 microliters deionized water, the contact angle of the water was measured, the drop contact angle was less than 30 ° before modification (i.e., the copper plate of S1), and 160 ° after modification (i.e., the abrasion-resistant super-hydrophobic surface of S3), as shown in fig. 12.
The contact angle of the drop was measured as 152 deg. using 400 mesh sandpaper repeatedly rubbed against the super-wetted surface of the copper plate, and then a 5 microliter drop of deionized water was used on the copper laser machined surface (see fig. 12).
The above examples are only some embodiments of the present invention, and are merely for illustrating the present invention, not for limiting the present invention, and those skilled in the art should not be able to make any changes, substitutions, modifications, etc. without departing from the spirit of the present invention.
Claims (10)
1. An abrasion-resistant super-wetted surface comprising a first region and a second region; the first region is a non-oxidation region, and the second region is an oxidation region; the thickness of the first area in the vertical direction of the laser oxidation abrasion-resistant super-wetting surface is not smaller than that of the second area; the second area comprises micro-nano rough metal and metal oxide; the second region area occupies 25% -100% of the wear resistant super wetting surface area.
2. The wear resistant super-wetted surface of claim 1, wherein the number of second regions is not less than 1, and wherein the shape of individual second regions is one of square, rectangular, triangular, diamond, circular, and hexagonal.
3. The wear resistant super wetting surface according to claim 1, wherein said micro-nano rough metal layer comprises a base metal, a melt cooled metal, sputtered metal particles, said metal oxide covering the micro-nano rough metal layer surface; the metal oxide comprises a first aggregation form and a second aggregation form, wherein the first aggregation form is a grass aggregation metal oxide; the metal oxide in the second aggregation form is a cauliflower-shaped aggregation metal oxide.
4. A wear resistant super wetting surface according to claim 3, characterised in that the grass-like aggregated metal oxide is agglomerated to a lesser extent than the cauliflower-like aggregated metal oxide; the thickness of the grass-like aggregated metal oxide in the vertical direction of the wear-resistant super-wetting surface is not greater than that of the cauliflower-like aggregated metal oxide.
5. A wear resistant super wetting surface according to claim 3, characterised in that said grass-like aggregated metal oxide comprises metal particle surface oxide and surface oxide of the base molten metal which solidifies upon re-cooling; the thickness of the surface oxide of the metal particles in the vertical direction of the wear-resistant super-wetting surface is not less than the thickness of the surface oxide of the substrate molten metal which is cooled and solidified again; the agglomeration degree of the surface oxide of the metal particles is not less than that of the surface oxide solidified by cooling the molten metal of the substrate.
6. A method for preparing an abrasion-resistant super-wetted surface, comprising the steps of:
Cleaning the metal piece, and then irradiating the surface of the metal piece with pulse laser according to a required pattern to form grass-like gathered metal oxide and cauliflower-like gathered metal oxide in a second area, so as to obtain the metal piece with the wear-resistant super-wetting surface; the power of the pulse laser is more than 0.1W; the irradiation rate of the pulse laser is 0.1-1000mm/s, and the pulse frequency of the pulse laser is 1 kHz-100 kHz; the beam spot diameter of the laser beam of the pulse laser is 10-500 mu m, and the number of irradiation cycles of the pulse laser is 1-50 times.
7. The method of claim 6, wherein the metal is one or more of copper, silver, aluminum, titanium, magnesium, iron, zinc, chromium, nickel, and alloys thereof; the atmosphere of the pulse laser is one or more of air, nitrogen, argon, helium and oxygen when the pulse laser irradiates.
8. The method of claim 6, wherein the distance between the laser adjacent lines when the pulsed laser irradiates the surface of the metal part is not greater than the spot diameter, and the difference between the distance between the laser adjacent lines when the pulsed laser irradiates the surface of the metal part and the spot diameter is less than 50 μm.
9. The method of producing an abrasion-resistant super-wetted surface according to claim 6, wherein the metal member containing the abrasion-resistant super-wetted surface is immersed in a modifying agent for low surface energy substance treatment; the modifier is more than one of fluorosilane, stearic acid, siloxane polysilane and polyvinyl fluoride; the soaking time is 10min to 12h.
10. The method of producing a wear-resistant super-wetted surface according to claim 6, wherein after cleaning the metal member, the surface of the metal member is covered with a wear-resistant phase material, and then pulse laser irradiation is performed; the physical wear-resistant phase material is more than one of silicon dioxide, diamond and silicon carbide.
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