CN112744783A - Preparation method of super-hydrophobic and super-oleophobic surface with micro-nano composite structure - Google Patents
Preparation method of super-hydrophobic and super-oleophobic surface with micro-nano composite structure Download PDFInfo
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- CN112744783A CN112744783A CN202110012365.6A CN202110012365A CN112744783A CN 112744783 A CN112744783 A CN 112744783A CN 202110012365 A CN202110012365 A CN 202110012365A CN 112744783 A CN112744783 A CN 112744783A
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 27
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 23
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000005530 etching Methods 0.000 claims abstract description 21
- 238000000151 deposition Methods 0.000 claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 14
- 239000010703 silicon Substances 0.000 claims abstract description 14
- 229910052709 silver Inorganic materials 0.000 claims abstract description 14
- 239000004332 silver Substances 0.000 claims abstract description 14
- 239000005046 Chlorosilane Substances 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 12
- -1 perfluoroalkyl chlorosilane Chemical compound 0.000 claims abstract description 11
- 239000000725 suspension Substances 0.000 claims abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000012545 processing Methods 0.000 claims abstract description 8
- 238000005516 engineering process Methods 0.000 claims abstract description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 18
- 229920002120 photoresistant polymer Polymers 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 8
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 5
- 239000008103 glucose Substances 0.000 claims description 5
- 238000001020 plasma etching Methods 0.000 claims description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000007385 chemical modification Methods 0.000 claims description 3
- 239000002270 dispersing agent Substances 0.000 claims description 3
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 claims description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 7
- 239000003921 oil Substances 0.000 abstract description 6
- 238000001259 photo etching Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 230000002265 prevention Effects 0.000 abstract description 2
- 244000020998 Acacia farnesiana Species 0.000 description 10
- 235000010643 Leucaena leucocephala Nutrition 0.000 description 10
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00444—Surface micromachining, i.e. structuring layers on the substrate
- B81C1/00492—Processes for surface micromachining not provided for in groups B81C1/0046 - B81C1/00484
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00523—Etching material
- B81C1/00547—Etching processes not provided for in groups B81C1/00531 - B81C1/00539
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
- B81C2201/0101—Shaping material; Structuring the bulk substrate or layers on the substrate; Film patterning
- B81C2201/0102—Surface micromachining
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- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention discloses a preparation method of a super-hydrophobic and super-oleophobic surface with a micro-nano composite structure. The method comprises the steps of firstly preparing a suspension micrometer column array on the surface of silicon by utilizing photoetching and deep silicon etching processes in a micro-nano processing technology, then depositing nano silver particles on the tops of the micrometer columns through silver mirror reaction, and utilizing O2And finally, carrying out low surface energy modification on the obtained micro-nano composite structure through perfluoroalkyl chlorosilane to obtain the super-hydrophobic and super-oleophobic functional surface. The micro/nano structure of the micro/nano composite structure prepared by the method has adjustable shape, height and density, has the advantages of simple operation, easy realization, low cost and the like, can obtain good mechanical performance, and has wide application prospect in the aspects of pollution prevention, self cleaning, water-oil separation and the like.
Description
Technical Field
The invention belongs to the technical field of micro-nano processing, and particularly relates to a preparation method of super-hydrophobic and super-oleophobic surfaces of a micro-nano composite structure.
Background
As a special wettability state, the super-hydrophobic and super-oleophobic surface has gained wide attention due to the huge application potential in the aspects of corrosion prevention, self-cleaning, water-oil separation, drag reduction and the like.
At present, researches on preparation of super-hydrophobicity are more, and the main preparation methods are mainly to perform chemical modification with low surface energy and construct a micron/nanometer high-roughness structure based on a Wenzel or Cassie model, wherein the Cassie model is easier to obtain a stable super-lyophobic effect due to the existence of an air interface in the structure. However, since the surface tension of oil is smaller than that of water, it is difficult to obtain super-amphiphobic properties only by low surface energy modification and conventional rough surface structure. Research shows that the introduction of the concave angle structures such as suspension, multistage and reentrant structures can enable low surface energy liquid such as oil to form liquid level bending between the structures so as to bring upward Laplace force, overcome Wenzel state energy barrier to form a solid-liquid-gas three-phase interface in a Cassie state, and have better lyophobic performance.
The Cassie model is excellent in lyophobic performance mainly due to an air layer in the structure, but is liable to cause collapse of the air layer due to external disturbance such as vibration, pressurization and the like to turn into a completely wetted Wenzel state. The composite nanostructure not only can stabilize Cassie state, but also can further improve amphiphobic performance.
The traditional nano structure composite method comprises spraying, self-assembly, phase separation and the like, wherein the surface with the micro-column structure is difficult to be uniformly coated to form a uniform film layer, so that the spraying and other methods are difficult to make the side wall of the micro-column smooth, and the side wall roughness can hinder the stability of Cassie state. Therefore, how to simply and conveniently load the nano-structure on the top of the micro-structure and make the nano-structure have a stable Cassie state is a problem which needs to be solved urgently at present.
Disclosure of Invention
The invention aims to provide a preparation method of a micro-nano composite structure, which is used for obtaining a stable super-amphiphobic functional surface.
The technical scheme adopted by the invention is as follows:
a method for preparing a super-hydrophobic and super-oleophobic surface of a micro-nano composite structure comprises the following steps:
a) preparing a column array of photoresist by using a micro-nano processing technology, and performing deep silicon etching to obtain a suspension micron column array;
b) carrying out anti-sticking treatment on the side wall and the bottom of the suspended micro-column array by using perfluoroalkyl chlorosilane;
c) inverting the array structure subjected to anti-sticking treatment to float in a silver mirror reaction mixed solution, and depositing nano silver particles on the top of the suspended micro-column;
d) using reactive ion etching techniques with O2Etching the photoresist by using the silver particles as a mask under certain flow and certain power by using the plasma to obtain a micro-nano composite structure;
e) depositing SiO on the surface of the micro-nano composite structure2In a vacuum system, perfluoroalkyl chlorosilane is used for carrying out chemical modification on the structure surface with low surface energy to obtain the super-hydrophobic and super-oleophobic surface.
Further, in the step a), the cross section of the column array is square, the line width is 10-50 μm, and the duty ratio is 1.2% -80%.
Furthermore, in the step a), the height of deep silicon etching is more than or equal to 5 μm.
Further, in the step b), the anti-sticking treatment specifically comprises the following steps: with O2Processing the suspended micron column array for 60s to form silicon hydroxyl on the side wall and the bottom of the suspended micron column array, wherein the hydroxyl cannot be formed on the top of the array by photoresist; and then placing the suspended micron column array into a vacuum drying dish, dripping 10 mu L of perfluoroalkyl chlorosilane, and standing for 20h to volatilize the perfluoroalkyl chlorosilane to the surface of the array.
Further, in the step c), a silver mirror reaction mixed solution is formed by adding 100mM glucose solution and 2 wt% of dispersant polyvinylpyrrolidone into a silver-ammonia complex formed by 100mM silver nitrate and 600mM ammonia water; the temperature for depositing the nano silver particles is 22-60 ℃, and the deposition time is 3-15 min.
Further, in the silver mirror reaction mixed solution, the volume ratio of ammonia water to silver nitrate is greater than or equal to 6, the volume ratio of glucose solution to silver nitrate is 0.2-1, and the volume ratio of polyvinylpyrrolidone to silver nitrate is 0.1-0.4.
Further, in said step d), O2The plasma flow is 10sccm, the power is 40W, the etching time is 100s, and the etching depth is 150 nm.
Further, in the step e), SiO2Deposition thickness of 20nm。
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, the overhanging micron square column array is prepared by utilizing photoetching and deep silicon etching methods, and compared with general column alignment, a special parallel channel of a square column can provide larger and stable Laplace force, so that the Cassie state is further stabilized.
(2) The method utilizes chemical deposition of silver mirror reaction, has good adaptability to uneven surfaces, and can effectively prevent reaction solution from entering through the fact that the micron columns after the side walls are anti-sticking are inversely suspended on the liquid level, so that the nano silver particles only grow on the top of the structure, the side walls are guaranteed to be smooth, and the Cassie state is convenient to stabilize.
(3) The invention can prepare the suspension nanostructure with high duty ratio by adjusting the reaction time of the silver mirror, not only can stabilize Cassie state for solid-liquid-gas three-phase line pinning, but also can further improve amphiphobic performance.
(4) The micro/nano composite structure prepared by the method has the advantages of adjustable shape, height and density of the micro/nano structure, simple operation, easy realization, low cost, large and uniform area and the like, can obtain good mechanical property, and has wide application prospect in the aspects of pollution prevention, self cleaning, water-oil separation and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a flow chart of the production process of the present invention;
FIG. 2 is an SEM plane and a cross-sectional view of a suspended micrometer square column prepared according to the present invention (b);
FIG. 3 is (a) SEM plane and (b) sectional view of a micro-nano composite structure prepared by the invention;
fig. 4 is a contact angle test chart of (a) water and (b) hexadecane of the micro-nano composite structure prepared by the invention.
In the figure: 1-photoresist, 2-silicon chip, 3-photoetching mask plate, 4-perfluoroalkyl chlorosilane monomolecular layer, 5-silver mirror reaction mixed solution and 6-nano silver particles.
Detailed Description
As shown in fig. 1, this embodiment provides a method for preparing a superhydrophobic and superoleophobic surface with a micro-nano composite structure, which includes the following specific steps:
1. preparation of suspended micrometer square column: a common silicon wafer 2(n or p type, resistivity, crystal orientation and the like have no requirements) is adopted to spin-coat photoresist 1, the speed is 4000r/s, the time is 40s, and the film thickness is 1.5 mu m. And taking a square photoetching mask plate 3 with the line width of 50 mu m and the period of 100 mu m for photoetching to obtain a photoresist square column with the line width of 50 mu m and the period of 100 mu m. Deep silicon etching is carried out by taking photoresist as mask and etching gas is SF6The protective gas is C4F8Depth 10 μm, resulting in a suspended micrometer square column array.
2. The bottom of the side wall of the micron square column is anti-sticking: the samples were first surface treated using an ICP-RIE (ULVAC, CE-300I) etching process: with O2Processing for 60s to enable the side wall and the bottom of the suspension structure to form silicon hydroxyl, wherein the top of the suspension structure is provided with the photoresist which cannot form hydroxyl; then the sample is put into a vacuum drying dish, 10 mu L of perfluoroalkyl chlorosilane is dripped in, and the sample is kept stand for 20h to be volatilized to the surface of the sample.
3. And (3) deposition of nano silver particles: in 1mL of AgNO3To (0.1M) was added 200. mu.L of NaOH solution (0.1M) to give a brown suspension, and then 6mL of NH was slowly added dropwise3H2O (0.6M) formed a clear silver ammine complex solution to which was added 400. mu.L of glucose (0.1M) solution and 200. mu.L of PVP as dispersant. And (3) inverting the sample subjected to the anti-sticking treatment in the step (2) to float on the liquid surface of the silver mirror reaction mixed solution 5, reacting for 7 minutes at the temperature of 50 ℃, and depositing the nano silver particles 6 with the diameter of about 80nm on the tops of the suspended micrometer square columns.
4. Preparing a nano composite structure: etching for 100s by using ICP-RIE (ULVAC, CE-300I) etching process and taking the nano silver particles 6 as a mask, wherein the etching gas is O2The gas flow is 10sccm, the power is 40W, the etching rate is 1.5nm/s, and the etching depth is 150 nm.
5. Preparing a super-amphiphobic surface: depositing SiO with about 20nm on the surface of the micro-nano composite structure by using a chemical vapor deposition method (PECVD, Plasma Enhanced Chemical Vapor Deposition (PECVD) system 80Plus)2. The samples were first surface treated using an ICP-RIE (ULVAC, CE-300I) etching process: with O2Processing for 60s to enable the side wall and the bottom of the suspension structure to form silicon hydroxyl, wherein the top of the suspension structure is provided with the photoresist which cannot form hydroxyl; then the sample is put into a vacuum drying dish, 10 mu L of perfluoroalkyl chlorosilane is dripped in, and the sample is kept stand for 20h to be volatilized to the surface of the sample. And (3) obtaining a functional surface of the micro-nano composite structure with super hydrophobicity and super oleophobicity, and measuring the water-oil contact angle of the functional surface, as shown in figure 4, the water contact angle is 159 degrees, and the hexadecane contact angle is 153 degrees.
Claims (8)
1. A preparation method of a super-hydrophobic and super-oleophobic surface with a micro-nano composite structure is characterized by comprising the following steps:
a) preparing a column array of photoresist by using a micro-nano processing technology, and performing deep silicon etching to obtain a suspension micron column array;
b) carrying out anti-sticking treatment on the side wall and the bottom of the suspended micro-column array by using perfluoroalkyl chlorosilane;
c) inverting the array structure subjected to anti-sticking treatment to float in a silver mirror reaction mixed solution, and depositing nano silver particles on the top of the suspended micro-column;
d) using reactive ion etching techniques with O2Etching the photoresist by using the silver particles as a mask under certain flow and certain power by using the plasma to obtain a micro-nano composite structure;
e) depositing SiO on the surface of the micro-nano composite structure2In a vacuum system, perfluoroalkyl chlorosilane is used for carrying out chemical modification on the structure surface with low surface energy to obtain the super-hydrophobic and super-oleophobic surface.
2. The method for preparing the superhydrophobic and superoleophobic surface with the micro-nano composite structure according to claim 1, characterized in that in step a), the cross section of the column array is square, the line width is 10-50 μm, and the duty ratio is 1.2% -80%.
3. The method for preparing the super-hydrophobic and super-oleophobic surface of the micro-nano composite structure according to claim 1, characterized in that in step a), the height of deep silicon etching is not less than 5 μm.
4. The method for preparing the superhydrophobic and superoleophobic surface of the micro-nano composite structure according to claim 1, characterized in that in step b), the anti-sticking treatment comprises the following specific steps: with O2Processing the suspended micron column array for 60s to form silicon hydroxyl on the side wall and the bottom of the suspended micron column array, wherein the hydroxyl cannot be formed on the top of the array by photoresist; and then placing the suspended micron column array into a vacuum drying dish, dripping 10 mu L of perfluoroalkyl chlorosilane, and standing for 20h to volatilize the perfluoroalkyl chlorosilane to the surface of the array.
5. The method for preparing the super-hydrophobic and super-oleophobic surface of the micro-nano composite structure according to claim 1, characterized in that in the step c), 100mM glucose solution and 2 wt% dispersant polyvinylpyrrolidone are added into a silver-ammonia complex formed by 100mM silver nitrate and 600mM ammonia water to form a silver mirror reaction mixed solution; the temperature for depositing the nano silver particles is 22-60 ℃, and the deposition time is 3-15 min.
6. The method for preparing the super-hydrophobic and super-oleophobic surface with the micro-nano composite structure according to claim 5, characterized in that in the silver mirror reaction mixed solution, the volume ratio of ammonia water to silver nitrate is greater than or equal to 6, the volume ratio of glucose solution to silver nitrate is 0.2-1, and the volume ratio of polyvinylpyrrolidone to silver nitrate is 0.1-0.4.
7. The method for preparing the super-hydrophobic and super-oleophobic surface of the micro-nano composite structure according to claim 1, characterized in that in step d), O is2The plasma flow is 10sccm, the power is 40W, the etching time is 100s, and the etching depth is 150 nm.
8. The method for preparing the super-hydrophobic and super-oleophobic surface of the micro-nano composite structure according to claim 1, characterized in that in step e), SiO is used2The deposition thickness was 20 nm.
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