CN115922091A - Method for rapidly preparing ultralyophobic surface - Google Patents
Method for rapidly preparing ultralyophobic surface Download PDFInfo
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- CN115922091A CN115922091A CN202310244081.9A CN202310244081A CN115922091A CN 115922091 A CN115922091 A CN 115922091A CN 202310244081 A CN202310244081 A CN 202310244081A CN 115922091 A CN115922091 A CN 115922091A
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- 238000000034 method Methods 0.000 title claims abstract description 49
- 238000012545 processing Methods 0.000 claims abstract description 23
- 230000008569 process Effects 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 15
- 230000004048 modification Effects 0.000 claims abstract description 9
- 238000012986 modification Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- XPBBUZJBQWWFFJ-UHFFFAOYSA-N fluorosilane Chemical compound [SiH3]F XPBBUZJBQWWFFJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002086 nanomaterial Substances 0.000 claims description 6
- 229910000838 Al alloy Inorganic materials 0.000 claims description 5
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000010276 construction Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 238000000861 blow drying Methods 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- KYIDJMYDIPHNJS-UHFFFAOYSA-N ethanol;octadecanoic acid Chemical compound CCO.CCCCCCCCCCCCCCCCCC(O)=O KYIDJMYDIPHNJS-UHFFFAOYSA-N 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 2
- 238000003754 machining Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 55
- 235000019483 Peanut oil Nutrition 0.000 description 6
- 239000000312 peanut oil Substances 0.000 description 6
- 230000003075 superhydrophobic effect Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 235000019198 oils Nutrition 0.000 description 4
- 238000002791 soaking Methods 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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Abstract
The invention relates to the field of special machining of ultralyophobic surfaces, and particularly provides a method for quickly preparing an ultralyophobic surface. The method has the advantages of simple operation, good universality, low cost, high efficiency and the like, and can realize the ultra-fast preparation of the ultra-lyophobic surface by a one-step method. In the processing process, the laser can not only construct a microstructure on the surface of a sample, but also promote the combination of the microstructure and a low-surface-energy substance and strengthen the modification effect of the low-surface-energy substance, so that the ultralyophobic surface can be obtained without modifying the processed sample with the low-surface-energy substance, and the ultralyophobic performance can be effectively improved, the preparation period is shortened and the preparation efficiency is improved.
Description
Technical Field
The invention relates to the field of special processing of an ultralyophobic surface, and particularly provides a method for quickly preparing an ultralyophobic surface based on a laser processing technology.
Background
The ultralyophobic surface refers to a surface on which liquid such as water, oil and the like has a contact angle of more than 150 degrees, and mainly comprises a superhydrophobic surface and an ultraoleophobic surface. The super-lyophobic surface can effectively prevent liquid such as water, oil and the like from being adhered, and has the characteristics of self-cleaning property, corrosion resistance, bacterial pollution resistance, icing and frosting resistance and the like, so the super-lyophobic surface has important application prospects in the fields of national defense and military industry, medical instruments, building materials and the like.
Firstly, constructing a proper micro or nano-scale microstructure on the surface of a substrate by using special processing technologies such as electrochemical etching, chemical etching, coating covering, plasma treatment, laser processing and the like to ensure that the surface obtains super-lyophilic property; and then, low-surface-energy substances such as stearic acid, fluorosilane, perfluorooctanoic acid and the like are attached to the surface with the microstructure by using methods such as coating, solution dipping and the like, so that the surface obtains super-lyophobic property. For example, CN201610008569.1 discloses a method for processing a superhydrophobic surface by an electro-hydraulic beam process, in which a microstructure is first constructed by an electro-hydraulic beam processing technique to make the surface superhydrophilic, and then a sample is soaked in a solution containing a low surface energy substance such as stearic acid or fluorosilane (referred to as a low surface energy solution for short) to obtain the superhydrophobic surface. CN201611191896.1 discloses a method for processing superhydrophobic surface by laser, which comprises constructing microstructure by femtosecond laser processing technique to make surface superhydrophilic, and soaking sample in fluorosilane solution to obtain superhydrophobic surface.
Although the above methods can prepare an ultralyophobic surface, in the existing processing method, after a microstructure is built on the surface of a sample, liquid such as water, oil and the like is completely spread on the sample, and the sample shows ultralyophilic properties with a contact angle less than 5 degrees, so that the processed sample needs to be soaked in a low surface energy solution for more than 20 minutes to complete the modification process of the low surface energy substance, so that the surface obtains ultralyophobic property. In addition, in the soaking process, the combination of the surface microstructure and the low surface energy substance is unstable, and the problems of poor durability, poor uniformity and the like of the surface super-lyophobic property are easily caused.
Therefore, the performance and the preparation efficiency of the super lyophobic surface are severely restricted by the existing preparation method of the super lyophobic surface, and the application and the popularization and the large-scale production of the super lyophobic surface are limited.
Disclosure of Invention
In order to solve the problems, the invention carries out laser processing on the sample in the low-surface solution, so that the laser, the sample material and the low-surface-energy substance interact with each other, and simultaneously completes the microstructure construction of the surface of the sample and the modification process of the low-surface-energy substance.
The invention provides a method for quickly preparing an ultralyophobic surface, which comprises the following steps:
s1, cleaning a sample to be processed and then drying the sample;
s2, immersing the sample in a low surface energy solution;
s3, laser processing is carried out on the sample immersed in the low surface energy solution by adopting laser with the power of more than or equal to 0.01W, and meanwhile, micro-nano structure construction and low surface energy modification of the surface of the sample are realized;
and S4, taking out the sample, and naturally airing or blow-drying to obtain the super lyophobic surface.
Preferably, the sample is aluminum, aluminum alloy, titanium, steel, glass, ceramic or graphene.
Preferably, the sample is ultrasonically cleaned with acetone, isopropanol and deionized water.
Preferably, the low surface energy solution is stearic acid ethanol solution, fluorosilane ethanol solution, perfluorooctanoic acid aqueous solution or other solution containing low surface energy substances.
Preferably, when the liquid level of the low surface energy solution is higher than the highest point of the sample but not more than 1mm, the wavelength of the laser is 315nm-1060nm, the repetition frequency is 1Hz-1MHz, the pulse width is 20fs-1ns, the focal length is 0.1mm-1000mm, the laser power is 0.01W-100W, the scanning speed is 0.01mm/s-100m/s, and the scanning distance is 0.001mm-10mm.
Preferably, when the liquid level of the low surface energy solution is higher than the highest point of the sample and exceeds 1mm, the wavelength of the laser is 315nm-1060nm, the repetition frequency is 1Hz-1MHz, the pulse width is 20fs-1ns, the focal length is 0.1mm-1000mm, the laser power is at least 1W, the scanning speed is 0.01mm/s-100m/s, and the scanning distance is 0.001mm-10mm.
Preferably, in S2 and S3, the sample may be placed horizontally or vertically.
Preferably, the laser is used to process the sample from directly above the sample when the sample is horizontally positioned.
Preferably, when the sample is vertically placed, the laser is used for processing the sample from the periphery of the sample.
Compared with the prior art, the invention can obtain the following beneficial effects:
the method has the advantages of simple operation, good universality, low cost, high efficiency and the like, and can realize the ultra-fast preparation of the ultra-lyophobic surface by a one-step method. In the processing process, the laser can not only build a microstructure on the surface of the sample, but also promote the combination of the microstructure and a low-surface-energy substance and strengthen the modification effect of the low-surface-energy substance, so that the super-lyophobic surface can be obtained without modifying the processed sample with the low-surface-energy substance, and the super-lyophobic performance can be effectively improved, the preparation period is shortened and the preparation efficiency is improved.
Drawings
FIG. 1 is a flow chart of a method for rapidly preparing an ultralyophobic surface according to an embodiment of the invention;
FIG. 2 is a schematic illustration of a process for rapidly preparing an ultralyophobic surface according to an embodiment of the invention;
FIG. 3 is a schematic illustration of a laser processing trajectory provided in accordance with an embodiment of the present invention;
FIG. 4 is a schematic illustration of a contact angle of a water droplet on an ultralyophobic surface provided in accordance with an embodiment of the invention;
figure 5 is a schematic illustration of the contact angle of a droplet of peanut oil on an ultralyophobic surface provided in accordance with an embodiment of the invention.
Wherein the reference numerals include:
Detailed Description
Hereinafter, embodiments of the present invention will be described with reference to the 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, detailed description thereof will not be repeated.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not to be construed as limiting the invention.
Fig. 1 illustrates a process for rapidly preparing an ultralyophobic surface provided according to an embodiment of the present invention.
Fig. 2 illustrates a process for rapidly preparing an ultralyophobic surface provided in accordance with an embodiment of the present invention.
As shown in fig. 1 and 2, in the embodiment of the present invention, the method for rapidly preparing an ultralyophobic surface is used for preparing an ultralyophobic surface on an aluminum alloy, and the method includes the following specific steps:
s1, the sample 4 to be processed can be made of metal, metal alloy or nonmetal materials, such as aluminum, titanium, steel, glass, ceramics, graphene and the like.
As an optional embodiment, the sample 4 is made of an aluminum alloy block, the sample 4 is ultrasonically cleaned by acetone, isopropanol and deionized water, oil stains and impurities on the surface of the sample 4 are removed, and the cleaned sample 4 is dried by nitrogen jet.
S2, preparing a stearic acid ethanol solution, a fluorosilane ethanol solution, a perfluorooctanoic acid aqueous solution or other solutions containing low-surface-energy substances as the low-surface-energy solution 2, and immersing the sample 4 in the low-surface-energy solution 2.
As an alternative example, a container 3 is used for containing a proper amount of 0.015mol/L perfluorooctanoic acid aqueous solution, a sample 4 is immersed in the low surface energy solution 2, and the liquid level of the low surface energy solution 2 is ensured to be higher than the highest point of the surface of the sample 4.
Fig. 3 illustrates a laser processing trace provided in accordance with an embodiment of the present invention.
As shown in fig. 3, S3, adjusting laser processing parameters of the laser 1, such as wavelength, repetition frequency, pulse width, focal length, power, scanning speed, scanning pitch, and the like, and performing laser processing on the sample 4 immersed in the low surface energy solution 2 along the laser processing track of fig. 3 by using the laser 1 with power greater than or equal to 0.01W to construct micro-nano structures, i.e., micro-and nano-scale structures.
As an alternative example, when the liquid level of the low surface energy solution 2 is higher than the highest point of the sample 4, but the height is not more than 1mm, the process parameters of the laser 1 need to be selected as follows: the wavelength is 315nm-1060nm, the repetition frequency is 1Hz-1MHz, the pulse width is 20fs-1ns, the focal length is 0.1mm-1000mm, the laser power is 0.01W-100W, the scanning speed is 0.01mm/s-100m/s, the scanning distance is 0.001mm-10mm, and a group of specific process parameters of the laser 1 are as follows: a wavelength of 1030nm, a repetition frequency of 1kHz, a pulse width of 250fs, a focal length of 500mm, a laser power of 0.5W, a scanning speed of 1mm/s, and a scanning pitch of 0.1mm.
When the liquid level of the low surface energy solution 2 is higher than the highest point of the sample 4 and exceeds the height by more than 1mm, the process parameters of the laser 1 need to be selected as follows: the wavelength is 315nm-1060nm, the repetition frequency is 1Hz-1MHz, the pulse width is 20fs-1ns, the focal length is 0.1mm-1000mm, the laser power is at least 1W, the scanning speed is 0.01mm/s-100m/s, the scanning distance is 0.001mm-10mm, and a group of specific process parameters of the laser 1 are given as follows: a wavelength of 1030nm, a repetition frequency of 1kHz, a pulse width of 250fs, a focal length of 500mm, a laser power of 2W, a scanning speed of 1mm/s, and a scanning pitch of 0.1mm.
In addition, the laser power and the scanning speed can be reasonably adjusted within a value range according to specific processing conditions and the material of the sample 4.
As an alternative example, the sample 4 may be placed in the low surface energy solution 2 in a horizontal or vertical manner, and when the sample 4 is placed horizontally, the laser 1 processes the sample 4 from right above the sample 4; when sample 4 was vertically placed, laser 1 was processed sample 4 all around by sample 4, with the vertical piece of placing the sample and can avoiding processing to produce sheltered from the problem of laser, the piece can sink or come-up under gravity or buoyancy, avoided 1 sheltering from of laser and the inhomogeneous condition of micro-nano structure.
And S4, taking out the processed sample 4, and blow-drying or naturally airing the sample 4 by using nitrogen jet to obtain the super-lyophobic property.
Fig. 4 illustrates a contact angle of a water droplet on an ultralyophobic surface provided in accordance with an embodiment of the present invention.
Figure 5 shows the contact angle of a droplet of peanut oil on an ultralyophobic surface provided in accordance with an embodiment of the invention.
As shown in fig. 4 and 5, a drop of water and a drop of peanut oil were respectively dropped onto the ultralyophobic surface of sample 4, which exhibited a contact angle of 160 ° for the drop of water and 152 ° for the drop of peanut oil, as measured by the instrument, while the contact angles of the original surface of sample 4 for the drop of water and the drop of peanut oil were both around 70 °.
The verification experiment shows that compared with the super lyophobic surface processed by the conventional method, the method can simultaneously realize the micro-nano structure construction and the low surface energy modification of the surface of the sample, namely the super lyophobic surface can be directly obtained after laser processing. Furthermore, the machined ultralyophobic surface has a contact angle of greater than 150 ° for both water droplets and peanut oil droplets.
The method has feasibility and superiority, can realize the ultra-fast preparation of the ultra-lyophobic surface by a one-step method, takes the sample 4 of an aluminum alloy with the specification of 5mm multiplied by 5mm as an example, and takes about 1 minute for the preparation by the method provided by the embodiment; the traditional method of processing first and then soaking is used for preparation, the total time consumption is about more than 21 minutes, and even more than 3 hours are needed.
While embodiments of the present invention have been shown and described above, it should be understood that the above embodiments are exemplary and should not be taken as limiting the invention. Variations, modifications, substitutions and alterations of the above-described embodiments may be made by those of ordinary skill in the art without departing from the scope of the present invention.
The above embodiments of the present invention should not be construed as limiting the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the claims of the present invention.
Claims (9)
1. A method for rapidly preparing an ultralyophobic surface is characterized by comprising the following steps:
s1, cleaning a sample to be processed and then drying the sample;
s2, immersing the sample in a low surface energy solution;
s3, laser processing is carried out on the sample immersed in the low surface energy solution by adopting laser with the power of more than or equal to 0.01W, and meanwhile, micro-nano structure construction and low surface energy modification of the surface of the sample are realized;
and S4, taking out the sample, and naturally airing or blow-drying to obtain the super lyophobic surface.
2. The method of rapidly preparing an ultralyophobic surface according to claim 1, wherein the sample is aluminum, aluminum alloy, titanium, steel, glass, ceramic, or graphene.
3. The method of rapidly preparing an ultralyophobic surface of claim 1, wherein the sample is ultrasonically cleaned with acetone, isopropyl alcohol, deionized water.
4. The method of rapidly preparing an ultralyophobic surface according to claim 1, wherein the low surface energy solution is stearic acid ethanol solution, fluorosilane ethanol solution, perfluorooctanoic acid aqueous solution, or other solution containing low surface energy substance.
5. The method of rapidly preparing an ultralyophobic surface according to claim 1, wherein the liquid level of the low surface energy solution is higher than the highest point of the sample, but not more than 1mm, the laser has a wavelength of 315nm to 1060nm, a repetition frequency of 1Hz to 1MHz, a pulse width of 20fs to 1ns, a focal length of 0.1mm to 1000mm, a laser power of 0.01W to 100W, a scanning speed of 0.01mm/s to 100m/s, and a scanning pitch of 0.001mm to 10mm.
6. The method of rapidly preparing an ultralyophobic surface according to claim 1, wherein the liquid level of the low surface energy solution is higher than the highest point of the sample, and when it exceeds 1mm, the laser has a wavelength of 315nm to 1060nm, a repetition frequency of 1Hz to 1MHz, a pulse width of 20fs to 1ns, a focal length of 0.1mm to 1000mm, a laser power of at least 1W, a scanning speed of 0.01mm/s to 100m/s, and a scanning pitch of 0.001mm to 10mm.
7. The method of rapidly preparing an ultralyophobic surface according to claim 1, wherein in S2 and S3, the sample may be placed horizontally or vertically.
8. The method of rapidly preparing an ultralyophobic surface according to claim 7, wherein the laser is used to process the sample from directly above the sample when the sample is horizontally placed.
9. The method of rapidly preparing an ultralyophobic surface according to claim 7, wherein the laser processes the sample from the periphery of the sample when the sample is vertically placed.
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-
2023
- 2023-03-15 CN CN202310244081.9A patent/CN115922091A/en active Pending
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