CN112744783B - 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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- CN112744783B CN112744783B CN202110012365.6A CN202110012365A CN112744783B CN 112744783 B CN112744783 B CN 112744783B CN 202110012365 A CN202110012365 A CN 202110012365A CN 112744783 B CN112744783 B CN 112744783B
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 24
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000005530 etching Methods 0.000 claims abstract description 20
- 239000000725 suspension Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000000151 deposition Methods 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
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 13
- 239000010703 silicon Substances 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 12
- 239000005046 Chlorosilane Substances 0.000 claims abstract description 11
- -1 perfluoroalkyl chlorosilane Chemical compound 0.000 claims abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 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 16
- 229920002120 photoresistant polymer Polymers 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 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
- 230000008021 deposition Effects 0.000 claims description 5
- 239000008103 glucose Substances 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
- 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
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 claims description 3
- 238000007385 chemical modification Methods 0.000 claims description 3
- 239000002270 dispersing agent Substances 0.000 claims description 3
- 238000007667 floating Methods 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 6
- 239000003921 oil Substances 0.000 abstract description 6
- 238000001259 photo etching Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 3
- 230000002265 prevention Effects 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
- 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
- 238000001020 plasma etching Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 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
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition 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
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
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 preparing a suspension micron column array on the silicon surface by photoetching and deep silicon etching processes in micro-nano processing technology, depositing nano silver particles on the tops of micron columns through silver mirror reaction, and utilizing O 2 And finally, carrying out low surface energy modification on the obtained micro-nano composite structure through perfluoroalkyl chlorosilane to obtain the super-hydrophobic super-oleophobic functional surface. 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 and the like, can obtain good mechanical properties, 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 materials with a micro-nano composite structure.
Background
The super-hydrophobic and super-oleophobic surface is taken as a special wettability state, and has great application potential in the aspects of corrosion prevention, self-cleaning, water-oil separation, drag reduction and the like, so that the super-hydrophobic and super-oleophobic surface has a great deal of attention.
At present, many researches on preparation of super-hydrophobic materials are carried out, and the main preparation method is to carry out chemical modification of 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. Researches show that the introduction of concave angle structures such as overhang structures, multilevel structures, reentrant structures and the like can lead the liquid with low surface energy such as oil to form liquid level bending between the structures so as to bring upward Laplace force, overcome the energy barrier of the Wenzel state and form a solid-liquid-gas three-phase interface, and be in the Cassie state so as to have better lyophobic performance.
The excellent lyophobic properties of the Cassie model are mainly due to the air layer in the structure, but due to external disturbances such as vibration, pressurization, etc., the air layer is easily caused to collapse to be converted into a completely infiltrated Wenzel state. The pinning of the composite nanostructure to the solid-liquid-gas three-phase line not only can stabilize the Cassie state, but also can further improve the amphiphobic performance.
The traditional nano-structure compounding method comprises spraying, self-assembly, phase separation and the like, wherein the surface with the micro-column structure is difficult to uniformly glue to form a uniform film layer, so that the spraying and other methods are difficult to enable the side wall of the micro-column to be smooth, and the roughness of the side wall can prevent the stability of a Cassie state. How to simply and conveniently load the nanostructure on top of the microstructure and make it have a stable Cassie state is a problem that 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 preparation method of a super-hydrophobic and super-oleophobic surface with a micro-nano composite structure comprises the following steps:
a) Preparing a column array of photoresist by utilizing a micro-nano processing technology, and performing deep silicon etching to obtain a suspension micron column array;
b) The sidewall and the bottom of the suspension micron column array are subjected to anti-sticking treatment by perfluoroalkyl chlorosilane;
c) Reversely floating the array structure subjected to the anti-sticking treatment in a silver mirror reaction mixed solution, and depositing nano silver particles on the top of the suspension micron column;
d) By reactive ion etching technique, using O 2 Etching photoresist by using silver particles as a mask under a certain flow and a certain power by using plasma to obtain a micro-nano composite structure;
e) Depositing SiO on the surface of the micro-nano composite structure 2 In a vacuum system, perfluoroalkyl chlorosilane is used for carrying out chemical modification of low surface energy on the structure surface to obtain the super-hydrophobic and super-oleophobic surface.
Further, in the step a), the cross section of the pillar array is square, the line width is 10-50 μm, and the duty ratio is 1.2% -80%.
Further, in the step a), the height of deep silicon etching is more than or equal to 5 mu m.
Further, in the step b), the specific steps of the anti-adhesion treatment are as follows: with O 2 Treating the suspension micron column array for 60s to enable the side wall and the bottom of the suspension micron column array to form silicon hydroxyl groups, wherein the top of the array is photoresist which cannot form hydroxyl groups; then placing the suspension micron column array into a vacuum drying dish, dripping 10 mu L of perfluoroalkyl chlorosilane, and standing for 20h to volatilize the array surface.
Further, in the step c), adding 100mM glucose solution and 2wt% of dispersing agent polyvinylpyrrolidone 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 nano silver particles is 22-60 ℃, and the deposition time is 3-15min.
Further, in the silver mirror reaction mixed solution, the volume ratio of ammonia water to silver nitrate is more 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 the step d), O 2 The plasma flow was 10sccm, the power was 40W, the etching time was 100s, and the etching depth was 150nm.
Further, in said step e), siO 2 The deposition thickness was 20nm.
Compared with the prior art, the invention has the following advantages:
(1) Compared with the common column alignment, the parallel channels special for square columns can provide larger and stable Laplace force, and further stabilize the Cassie state.
(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 inverted suspension of the micron column on the liquid level after the side wall is anti-sticking, so that nano silver particles only grow on the top of the structure, the side wall is ensured to be smooth, and the Cassie state is convenient to stabilize.
(3) According to the invention, the high-duty-ratio suspension nanostructure can be prepared by adjusting the reaction time of the silver mirror, so that the Cassie state can be stabilized by pinning a solid-liquid-gas three-phase line, and the amphiphobic performance can be further improved.
(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 properties, 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 that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method of making the present invention;
FIG. 2 is a (a) SEM plan and (b) cross-sectional view of a suspended micron square column prepared according to the invention;
FIG. 3 is a (a) SEM plan and (b) cross-sectional view of a micro-nano composite structure prepared according to the present invention;
FIG. 4 is a graph showing the contact angle of (a) water and (b) hexadecane of the micro-nano composite structure prepared by the invention.
In the figure: 1-photoresist, 2-silicon wafer, 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, the embodiment provides a preparation method of a super-hydrophobic and super-oleophobic surface with a micro-nano composite structure, which specifically comprises the following preparation steps:
1. preparation of overhanging micrometer square columns: the photoresist 1 is spin-coated by adopting a common silicon wafer 2 (n or p type, no requirement on resistivity, crystal orientation and the like), the speed is 4000r/s, the time is 40s, and the film thickness is 1.5 mu m. And (5) taking a square photoetching mask plate 3 with a line width of 50 microns and a period of 100 microns for photoetching to obtain a square photoresist column with a line width of 50 microns and a period of 100 microns. Deep silicon etching with photoresist as mask and SF as etching gas 6 The protective gas is C 4 F 8 The depth was 10 μm, resulting in an array of overhanging micrometer square pillars.
2. Adhesion prevention of the bottom of the side wall of the micrometer square column: the samples were first surface treated using an ICP-RIE (ULVAC, CE-300I) etching process: with O 2 Treating for 60s to enable the side wall and the bottom of the overhang structure to form silicon hydroxyl, and enabling the photoresist at the top of the overhang structure to not form hydroxyl; then, the sample was placed in a vacuum drying dish, 10. Mu.L of perfluoroalkyl chlorosilane was dropped, and left to stand for 20 hours to volatilize to the surface of the sample.
3. Nano silver particle deposition: agNO in 1mL 3 200. Mu.L of NaOH solution (0.1M) was added to (0.1M) to give a brown suspension, and 6mL of NH was slowly added dropwise 3 H 2 O (0.6M) forms a clear silver ammonia complex solution to which 400. Mu.L glucose (0.1M) solution and 200. Mu.L PVP as a dispersant were added. And (3) reversely floating the sample subjected to the anti-sticking treatment in the step (2) on the liquid surface of the silver mirror reaction mixed solution (5), reacting for 7 minutes at the temperature of 50 ℃, and depositing nano silver particles (6) with the diameter of about 80nm on the top of the suspended micron square column.
4. Preparing a nano composite structure: etching with nanometer silver particles 6 as mask for 100s by ICP-RIE (ULVAC, CE-300I) etching process with etching gas as O 2 The gas flow was 10sccm, the power was 40W, the etching rate was 1.5nm/s, and the etching depth was 150nm.
5. Super-amphiphobic surfacePreparation: depositing SiO of about 20nm on the surface of the micro-nano composite structure by chemical vapor deposition (PECVD, plasmalabSystem Plus) 2 . The samples were first surface treated using an ICP-RIE (ULVAC, CE-300I) etching process: with O 2 Treating for 60s to enable the side wall and the bottom of the overhang structure to form silicon hydroxyl, and enabling the photoresist at the top of the overhang structure to not form hydroxyl; then, the sample was placed in a vacuum drying dish, 10. Mu.L of perfluoroalkyl chlorosilane was dropped, and left to stand for 20 hours to volatilize to the surface of the sample. The functional surface of the micro-nano composite structure with super-hydrophobic and super-oleophobic is obtained, and the water-oil contact angle is measured, and is shown in figure 4, wherein the water contact angle is 159 degrees, and the hexadecane contact angle is 153 degrees.
Claims (5)
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 utilizing a micro-nano processing technology, and performing deep silicon etching to obtain a suspension micron column array;
b) The sidewall and the bottom of the suspension micron column array are subjected to anti-sticking treatment by perfluoroalkyl chlorosilane; the anti-sticking treatment comprises the following specific steps: with O 2 Treating the suspension micron column array for 60s to enable the side wall and the bottom of the suspension micron column array to form silicon hydroxyl groups, wherein the top of the array is photoresist which cannot form hydroxyl groups; then placing the suspension 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;
c) Reversely floating the array structure subjected to the anti-sticking treatment in a silver mirror reaction mixed solution, and depositing nano silver particles on the top of the suspension micron column; adding 100mM glucose solution and 2wt% of dispersing agent polyvinylpyrrolidone into a silver ammonia complex formed by 100mM silver nitrate, 100mM sodium hydroxide solution and 600mM ammonia water to form a silver mirror reaction mixed solution, wherein the volume ratio of the ammonia water to the silver nitrate in the silver mirror reaction mixed solution is more than or equal to 6, the volume ratio of the glucose solution to the silver nitrate is 0.2-1, and the volume ratio of the polyvinylpyrrolidone to the silver nitrate is 0.1-0.4; the temperature for depositing nano silver particles is 22-60 ℃, and the deposition time is 3-15min;
d) By means of reactive ion etchingBy O 2 Etching photoresist by using silver particles as a mask under a certain flow and a certain power by using plasma to obtain a micro-nano composite structure;
e) Depositing SiO on the surface of the micro-nano composite structure 2 In a vacuum system, perfluoroalkyl chlorosilane is used for carrying out chemical modification of low surface energy on the structure surface to obtain the super-hydrophobic and super-oleophobic surface.
2. The method for preparing the super-hydrophobic and super-oleophobic surface of the micro-nano composite structure according to claim 1, wherein 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%.
3. The method for preparing the super-hydrophobic and super-oleophobic surface of the micro-nano composite structure according to claim 1, wherein in the step a), the deep silicon etching height is more than or equal to 5 μm.
4. The method for preparing a super-hydrophobic and super-oleophobic surface of a micro-nano composite structure according to claim 1, wherein in the step d), O 2 The plasma flow was 10sccm, the power was 40W, the etching time was 100s, and the etching depth was 150nm.
5. The method for preparing a super-hydrophobic and super-oleophobic surface of a micro-nano composite structure according to claim 1, wherein in the step e), siO 2 The deposition thickness was 20nm.
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CN113336185A (en) * | 2021-05-21 | 2021-09-03 | 大连理工大学 | Method for processing trans-scale micro-nano structure integrated with nano raised array |
CN113634293B (en) * | 2021-08-09 | 2023-02-28 | 复旦大学 | Light-operated all-inorganic EWOD device |
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