CN106423789B - A kind of durability anti-ice super-hydrophobic coat and preparation method thereof - Google Patents
A kind of durability anti-ice super-hydrophobic coat and preparation method thereof Download PDFInfo
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- CN106423789B CN106423789B CN201610934541.0A CN201610934541A CN106423789B CN 106423789 B CN106423789 B CN 106423789B CN 201610934541 A CN201610934541 A CN 201610934541A CN 106423789 B CN106423789 B CN 106423789B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/002—Pretreatement
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
- B05D7/52—Two layers
- B05D7/54—No clear coat specified
- B05D7/544—No clear coat specified the first layer is let to dry at least partially before applying the second layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2202/00—Metallic substrate
- B05D2202/10—Metallic substrate based on Fe
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2301/00—Inorganic additives or organic salts thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2350/00—Pretreatment of the substrate
- B05D2350/30—Change of the surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2507/00—Polyolefins
- B05D2507/01—Polyethylene
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- Life Sciences & Earth Sciences (AREA)
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- Wood Science & Technology (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Paints Or Removers (AREA)
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Abstract
The invention discloses a kind of durability anti-ice super-hydrophobic coat and preparation methods.It is made of bottom metal trench structure, intermediate macromolecule layer, top nano particle-polymer compound layer, using smooth steel as substrate, one layer of pure polymeric coating layer is coated after laser ablation groove structure, then spray on polymer-nano-composite coating is obtained, firstly, etching regular groove structure in smooth steel surface using laser；Then steel are subjected to O2After corona treatment, the ultra high molecular polyethylene and drying and forming-film of pyrolytic coating molten state；Finally, spraying ultra high molecular polyethylene and dewatering nano Al2O3Mixture, coating needed for being obtained after dry.Super-hydrophobic coat of the present invention has preferable mechanical stability and environmental persistence, and has excellent anti-ice performance.
Description
Technical field
The invention belongs to Material Field, it is related to a kind of durability anti-ice super-hydrophobic coat and preparation method thereof.
Background technique
Lotus leaf surface has to the extreme of water not wellability, referred to as super-hydrophobic phenomenon in nature.People pass through research
It was found that lotus leaf surface has the second level hierarchical structure of micron, nanometer, and surface covers the wax of a layered low-surface energy, so
Has ultra-hydrophobicity.Therefore, this hierarchical structure and the modification of the low-surface-energy in later period are prepared by various modes, can be obtained
Bionic super-hydrophobic interface.
Super-hydrophobic interface because of its excellent water resistant, hydrophobic performance, under water drag reduction, self-cleaning surface, metal protection and
There is huge application prospect in anti-icing anti-ice field.Main problem existing for super-hydrophobic coat is fragile surface texture at present.Though
The mode for so preparing super-hydrophobic interface is varied, but in very light extraneous scraping, surface texture can be destroyed, from
And super-hydrophobicity is lost, this is the bottleneck problem for restricting its a wide range of actual industrial.
Peng etc. is prepared for super-hydrophobic coat (the Chemically Stable and with wear-resisting property in surface of pure aluminum
Mechanically Durable Superamphiphobic Aluminum Surface with a Micro/Nanoscale
Binary Structure,ACS Appl. Mater. Interfaces, 2014,6 (17), pp 15188-15197).
They polish fine aluminium, after excusing from death cleaning, are put into the HCl solution of 2.5 M and perform etching, and then will be put into after coating drying
Hydro-thermal reaction is carried out in 120 °C of autoclave, to obtain interface micro nano structure；Finally, coating leaching is placed in perfluor silicon
It is modified that surface is carried out in alkane, obtains super-hydrophobic coat.This mode is more stringent to the restriction of substrate type, can only be in aluminium alloy table
Face carries out.Simultaneously as needing hydro-thermal reaction to carry out surface micronano, therefore there are strict requirements to sample size, size.
C.P.Wong seminar is successfully prepared for the super-hydrophobic coat (Mechanically with certain mechanical stability on silicon wafer
Robust superhydrophobicity on hierarchically structured Si surfaces,
Nanotechnology 21 (2010) 155705).They utilize H2O2With the mode of HF acid collaboration etching, prepared in Si on piece
Nanostructure out, and carried out friction testing.Although having certain mechanical stability, it is on relatively smooth rag
The friction of progress, and super-hydrophobicity is just lost after 25 cm of maximum friction, therefore stability still needs to improve.
Summary of the invention
The purpose of the present invention is to provide a kind of durability anti-ice super-hydrophobic coat and preparation method thereof, interface bottom gold
Belong to groove structure, intermediate macromolecule layer, top nano particle-polymer compound layer composition.The super-hydrophobic painting of durability anti-ice
Layer obtains undercut structure by handling the steel after sanding and polishing using laser；Then by the poly- second of supra polymer
It is dry after alkene solution spraying to groove structure surface, obtain intermediate macromolecule layer；Finally, by ultra high molecular polyethylene and being modified thin
Water Al2O3The mixture of nano particle is sprayed in substrate, obtains top nano particle-polymer compound layer.The coating is by outer
Still there is super-hydrophobicity and excellent anti-ice effect after boundary's abrasion.
The technical solution for realizing the aim of the invention is as follows:
A kind of durability anti-ice super-hydrophobic coat, by portion's metal valley structure, intermediate macromolecule layer, top nano particle-
Polymer compound layer composition.
Further, the metal valley structure is to utilize the steel groove structure after laser sanding and polishing；The groove
Concave structure depth is 200 ~ 300 μm, and width is 50 ~ 150 μm；Convex structure width is 100 ~ 200 μm.
The macromolecule layer is will to be dried to obtain after ultra high molecular polyethylene solution spraying to groove structure surface；Described
Ultra high molecular polyethylene molecular weight is 5000000, and spraying solvent for use is decahydronaphthalenes.
The nanometer Al2O3Grain diameter is 50 ~ 100 nm, and hydrophobic treatment is that nano particle is immersed in 0.05 ~ 0.08
In the ethanol solution of the heptadecafluorodecyl triethoxysilane of mol/L, soaking temperature is 50 ~ 60 °C, and soaking time is 3 ~ 4 h.
The preparation method of above-mentioned durability anti-ice super-hydrophobic coat, comprising the following steps:
1) steel after sanding and polishing are handled using laser, obtains undercut structure；
2) will be dry after ultra high molecular polyethylene solution spraying to groove structure surface, obtain intermediate macromolecule layer；
3) by ultra high molecular polyethylene and modified hydrophobic Al2O3The mixture of nano particle is sprayed in substrate, obtains top
Nano particle-polymer compound layer.
The concentration of the ultra high molecular polyethylene solution is 2 ~ 5 g/L, and spraying temperature is 150 °C.
The dewatering nano Al2O3The concentration of particle is 20 ~ 40 g/L, and ultra-high molecular weight polyethylene concentration is 6 ~ 10 g/
L, spraying temperature are 150 °C.
Compared with prior art, its remarkable advantage of the invention are as follows: 1) with the excellent mechanical stability of ultra high molecular polyethylene
Mechanical support is provided for nano particle, coating has good wearability；2) this hair does not want size, the shape of base material
It asks, it can be achieved that preparation on a large scale；3) present invention has excellent anti-ice performance.
Detailed description of the invention
Fig. 1 is the water droplet contact angle of 1 durability anti-ice super-hydrophobic coat of embodiment, roll angle.
Fig. 2 is the water droplet contact angle after the abrasion of 1 durability anti-ice super-hydrophobic coat of embodiment, roll angle.
Fig. 3 is the icing conditions comparison diagram of 1 coating of embodiment.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
Embodiment 1
(1) steel obtain groove structure with laser treatment, concave structure depth is 250 μm, and width is after polishing
100 μm；Convex structure width is 120 μm；
(2) after the sample clean for obtaining step (1), concentration is molten for the decahydronaphthalenes of 4 g/L ultra high molecular polyethylenes
Liquid is sprayed into drying behind groove structure surface, obtains intermediate macromolecule layer.
(3) Al for being 70 nm by partial size2O3Particle is immersed in the second of the heptadecafluorodecyl triethoxysilane of 0.06 mol/L
In alcoholic solution, soaking temperature is 55 °C, and soaking time is 3.5 h.
(4) the dewatering nano Al for obtaining step (3)2O3Particle, ultra high molecular polyethylene are added in decahydronaphthalenes, keep
Al2O3Concentration is 35 g/L, and ultra-high molecular weight polyethylene concentration is 8 g/L.Above-mentioned be mixed and heated to after 150 °C is sprayed on step
Suddenly dry on coating described in (2), obtain top nano particle-polymer compound layer.
It is prepared on coating, water drop static contact angle reaches 160 °, and roll angle is 2 °, as shown in Figure 1.5kPa,
It is polished after 2 m on 200# sand paper, contact angle is 155 °, roll angle is 5 °, as shown in Figure 2.After friction testing, it is placed in -20 °
C, the condensation of 90% humidity freezes under test environment, and coating surface does not occur apparent frost, illustrates that coating has excellent anti-ice
Performance, as shown in Figure 3.
Embodiment 2
(1) steel obtain groove structure with laser treatment, concave structure depth is 200 μm, and width is after polishing
150 μm；Convex structure width is 100 μm；
(2) after the sample clean for obtaining step (1), concentration is molten for the decahydronaphthalenes of 5 g/L ultra high molecular polyethylenes
Liquid is sprayed into drying behind groove structure surface, obtains intermediate macromolecule layer.
(3) Al for being 50 nm by partial size2O3Particle is immersed in the second of the heptadecafluorodecyl triethoxysilane of 0.07 mol/L
In alcoholic solution, soaking temperature is 50 °C, and soaking time is 4 h.
(4) the dewatering nano Al for obtaining step (3)2O3Particle, ultra high molecular polyethylene are added in decahydronaphthalenes, keep
Al2O3Concentration is 40 g/L, and ultra-high molecular weight polyethylene concentration is 6 g/L.Above-mentioned be mixed and heated to after 150 °C is sprayed on step
Suddenly dry on coating described in (2), obtain top nano particle-polymer compound layer.
It is prepared on coating, water drop static contact angle reaches 155 °, and roll angle is 4 °.It is beaten on 5kPa, 200# sand paper
After grinding 2 m, contact angle is 153 °, roll angle is 8 °.After friction testing, it is placed in the condensation icing test of -20 °C, 90% humidity
Under environment, coating surface does not occur apparent frost, illustrates that coating has excellent anti-ice performance.
Embodiment 3
(1) steel obtain groove structure with laser treatment, concave structure depth is 300 μm, and width is after polishing
50 μm；Convex structure width is 200 μm；
(2) after the sample clean for obtaining step (1), concentration is molten for the decahydronaphthalenes of 3 g/L ultra high molecular polyethylenes
Liquid is sprayed into drying behind groove structure surface, obtains intermediate macromolecule layer.
(3) Al for being 90 nm by partial size2O3Particle is immersed in the second of the heptadecafluorodecyl triethoxysilane of 0.08 mol/L
In alcoholic solution, soaking temperature is 60 °C, and soaking time is 3 h.
(4) the dewatering nano Al for obtaining step (3)2O3Particle, ultra high molecular polyethylene are added in decahydronaphthalenes, keep
Al2O3Concentration is 30 g/L, and ultra-high molecular weight polyethylene concentration is 8 g/L.Above-mentioned be mixed and heated to after 150 °C is sprayed on step
Suddenly dry on coating described in (2), obtain top nano particle-polymer compound layer.
It is prepared on coating, water drop static contact angle reaches 154 °, and roll angle is 3 °.It is beaten on 5kPa, 200# sand paper
After grinding 2 m, contact angle is 151 °, roll angle is 4 °.After friction testing, it is placed in the condensation icing test of -20 °C, 90% humidity
Under environment, coating surface does not occur apparent frost, illustrates that coating has excellent anti-ice performance.
Comparative example 1
(1) steel obtain groove structure with laser treatment, concave structure depth is 200 μm, and width is after polishing
150 μm；Convex structure width is 100 μm；
(2) after the sample clean for obtaining step (1), concentration is molten for the decahydronaphthalenes of 2 g/L ultra high molecular polyethylenes
Liquid is sprayed into drying behind groove structure surface, obtains intermediate macromolecule layer.
(3) Al for being 50 nm by partial size2O3Particle is immersed in the second of the heptadecafluorodecyl triethoxysilane of 0.05 mol/L
In alcoholic solution, soaking temperature is 550 °C, and soaking time is 3.5 h.
(4) the dewatering nano Al for obtaining step (3)2O3Particle, ultra high molecular polyethylene are added in decahydronaphthalenes, keep
Al2O3Concentration is 20 g/L, and ultra-high molecular weight polyethylene concentration is 7 g/L.Above-mentioned be mixed and heated to after 150 °C is sprayed on step
Suddenly dry on coating described in (2), obtain top nano particle-polymer compound layer.
It is prepared on coating, water drop static contact angle reaches 130 °, does not have ultra-hydrophobicity.Be placed in -20 °C,
The condensation of 90% humidity freezes under test environment, and apparent frost occurs in coating surface, illustrates that coating does not have anti-ice performance.
Comparative example 2
(1) steel obtain groove structure with laser treatment, concave structure depth is 300 μm, and width is after polishing
150 μm；Convex structure width is 120 μm；
(2) after the sample clean for obtaining step (1), concentration is molten for the decahydronaphthalenes of 2 g/L ultra high molecular polyethylenes
Liquid is sprayed into drying behind groove structure surface, obtains intermediate macromolecule layer.
(3) Al for being 100 nm by partial size2O3Particle is immersed in the heptadecafluorodecyl triethoxysilane of 0.06 mol/L
In ethanol solution, soaking temperature is 55 °C, and soaking time is 3.5 h.
(4) the dewatering nano Al for obtaining step (3)2O3Particle, ultra high molecular polyethylene are added in decahydronaphthalenes, keep
Al2O3Concentration is 25 g/L, and ultra-high molecular weight polyethylene concentration is 10 g/L.By it is above-mentioned be mixed and heated to 150 °C after be sprayed on
It is dry on coating described in step (2), obtain top nano particle-polymer compound layer.
It is prepared on coating, water drop static contact angle reaches 100 °, does not have ultra-hydrophobicity., be placed in -20 °C,
The condensation of 90% humidity freezes under test environment, and apparent frost occurs in coating surface, illustrates that coating does not have anti-ice performance.
Claims (7)
1. a kind of durability anti-ice super-hydrophobic coat, it is characterised in that: the coating is by bottom metal trench structure, intermediate macromolecule
Layer, top nano particle-polymer compound layer composition, the nano particle-polymer compound layer are dewatering nano Al2O3Particle
With ultra high molecular polyethylene composite coating；The nanometer Al2O3Grain diameter be more than or equal to 50, less than 100 nm, it is hydrophobic
Processing is the ethyl alcohol that nano particle is immersed in the heptadecafluorodecyl triethoxysilane greater than 0.05, less than or equal to 0.08 mol/L
In solution, soaking temperature is 50 ~ 60 °C, and soaking time is 3 ~ 4 h.
2. durability anti-ice super-hydrophobic coat according to claim 1, it is characterised in that: the metal valley structure is benefit
With the steel groove structure after laser sanding and polishing.
3. durability anti-ice super-hydrophobic coat according to claim 1, it is characterised in that: the metal valley structure are as follows:
Concave structure, depth are 200 ~ 300 μm, and width is 50 ~ 150 μm；Convex structure, width are 100 ~ 200 μm.
4. durability anti-ice super-hydrophobic coat according to claim 1, it is characterised in that: the macromolecule layer is by superelevation
It is dried to obtain after molecular polyethylene solution spraying to groove structure surface；The ultra high molecular polyethylene molecular weight is
5000000, spraying solvent for use is decahydronaphthalenes.
5. a kind of preparation method of durability anti-ice super-hydrophobic coat described in claim 1, it is characterised in that including following step
It is rapid:
1) steel after sanding and polishing are handled using laser, obtains undercut structure；
2) then will be dry after ultra high molecular polyethylene solution spraying to groove structure surface, obtain intermediate macromolecule layer；
3) by ultra high molecular polyethylene and modified hydrophobic Al2O3The mixture of nano particle is sprayed in substrate, obtains top nanometer
Particle-polymer compound layer.
6. the preparation method of durability anti-ice super-hydrophobic coat according to claim 5, it is characterised in that: the superelevation
The concentration of molecular polyethylene solution is 2 ~ 5 g/L, and spraying temperature is 150 °C.
7. the preparation method of durability anti-ice super-hydrophobic coat according to claim 5, it is characterised in that: described is hydrophobic
Nanometer Al2O3The concentration of particle is 20 ~ 40 g/L, and ultra-high molecular weight polyethylene concentration is 6 ~ 10 g/L, and spraying temperature is 150 °
C。
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| CN107267030B (en) * | 2017-07-26 | 2019-10-25 | 弘大科技（北京）股份公司 | A kind of super hydrophobic coating and its preparation and construction method |
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| CN111229565A (en) * | 2018-11-29 | 2020-06-05 | 南京理工大学 | Preparation method of magnetic super-hydrophobic surface |
| CN110694875A (en) * | 2019-11-15 | 2020-01-17 | 南京理工大学 | Method for obtaining super-hydrophobic surface of stepped layered structure |
| CN113145418A (en) * | 2020-01-07 | 2021-07-23 | 中国石油天然气集团有限公司 | Preparation method of super-hydrophobic material and super-hydrophobic material |
| CN112072005A (en) * | 2020-08-28 | 2020-12-11 | 昆山宝创新能源科技有限公司 | Aluminum-plastic film and preparation method and application thereof |
| CN114836725B (en) * | 2022-05-06 | 2023-10-13 | 上海海事大学 | Inorganic super-hydrophobic anti-icing coating structure for low-temperature steel and preparation method thereof |
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