CN105689236A - Preparing method for aluminum surface super-hydrophobic coating with micro-nano composite structure - Google Patents
Preparing method for aluminum surface super-hydrophobic coating with micro-nano composite structure Download PDFInfo
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- CN105689236A CN105689236A CN201610073380.0A CN201610073380A CN105689236A CN 105689236 A CN105689236 A CN 105689236A CN 201610073380 A CN201610073380 A CN 201610073380A CN 105689236 A CN105689236 A CN 105689236A
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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
- B05D5/083—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 involving the use of fluoropolymers
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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
- B05D3/02—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 by baking
- B05D3/0254—After-treatment
- B05D3/0272—After-treatment with ovens
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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
- B05D3/10—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 by other chemical means
- B05D3/102—Pretreatment of metallic substrates
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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
- B05D2202/00—Metallic substrate
- B05D2202/20—Metallic substrate based on light metals
- B05D2202/25—Metallic substrate based on light metals based on Al
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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
- B05D2350/33—Roughening
- B05D2350/35—Roughening by chemical means
Abstract
The invention discloses a preparing method for an aluminum surface super-hydrophobic coating with a micro-nano composite structure. The method mainly comprises the steps that firstly, an aluminum sheet is ultrasonically cleaned for 10 min through acetone and methylbenzene and then flushed thoroughly through distilled water, and the aluminum sheet is dried in an oven at the temperature being 100 DEG C; secondly, the cleaned and dried aluminum sheet is immersed in an acid etching agent to be etched, and an aluminum surface with a micron rough structure is obtained; thirdly, after the etched aluminum sheet is ultrasonically cleaned thoroughly, the aluminum sheet is immersed in a nano particle solution, and after the aluminum sheet is treated at the high temperature, an aluminum surface with a micro-nano composite rough structure is obtained; and fourthly, after low-surface-energy fluorosilicone modified polyester resin is sprayed to the aluminum surface with the micro-nano composite rough structure, an aluminum surface with super-hydrophobic performance can be obtained. The super-hydrophobic aluminum sheet prepared through the preparing method has the superior icing preventing performance and very good mechanical strength and can be applied to an air conditioner heat exchange sheet, and frosting and icing of the heat exchange sheet are effectively restrained.
Description
Technical field
The present invention relates to the preparation field of super hydrophobic surface, the preparation method being specifically related to a kind of aluminum surface super hydrophobic coating with micro-nano compound structure。
Background technology
Air-conditioning heats at low ambient temperatures, and owing to outer machine is placed on outdoor, the moisture in outdoor air can in the fin frosting of condenser, long ice crystal rolls up ice, being easily caused the vent passages blocking of fin, condenser heat exchange efficiency reduces, and affects the whole heating effect of air-conditioning。
Since " lotus leaf effect " finds, super hydrophobic surface is widely studied because having excellent properties。Research shows, super hydrophobic surface, except the self_cleaning effect with excellence, also has the performances such as excellent antifog, ice-covering-proof, anticorrosive, drag reduction。Super hydrophobic surface has good deicing properties, and its principle can be attributed to not-easy-to-freeze and be prone to deicing。Owing to super hydrophobic surface has the hydrophobicity of excellence, water is spherical distribution at coating surface, reduces the contact area of water and the surface of solids, heat transfer area between water droplet and solid is reduced, rate of heat transfer reduces, and therefore water exists coating surface in liquid form and is extended, and freezing time extends。It two is that the globule and the solid surface-attached power of liquid is little, and minimum inclination angle and external force just can allow water droplet tumble before icing。" air cushion " on super-hydrophobic coat surface can also reduce the contact area of ice and solid, reduces the adhesive force of ice and surface so that freezes and is easier to remove。
Structure and chemical composition research to lotus leaf surface find, constitute super hydrophobic surface and need to possess two key elements, and first is that the coarse structure needing micro-nano increases surface roughness；Second is the need for low-surface energy substance drops low-surface-energy。The preparation method being usually used in super hydrophobic surface has chemical etching method, chemical deposition, method of electrostatic spinning, template, sol-gal process, self assembly and LBL self-assembly method, plasma processing etc.。Wherein chemical etching method has that simple to operate, quick, reagent is cheap, large area the advantage such as can prepare, and has been widely used in the preparation of super hydrophobic surface。
In order to obtain the surface with micro-nano compound coarse structure, the present invention adopts two-step method that aluminium flake is processed。Initially with acid etch agent, aluminium flake is performed etching, obtain the surface with micron scale construction, then again at one layer of nanoparticle of etching surface dip-coating, obtain the surface with micro-nano compound coarse structure, micron order rough surface compared to single acid etch, its ultra-hydrophobicity is better, and anti-icing performance is more excellent。
Summary of the invention
In order to solve the frosting ice formation issues of heat sink of air conditioner, the preparation method that the invention provides a kind of aluminum surface super hydrophobic coating with micro-nano compound structure。By the structure of Folium Nelumbinis it can be seen that structure super hydrophobic surface need to possess micro-nano compound coarse structure, aluminium flake of the present invention adopts the method that salt acid etch and nanoparticle dip-coating combine to build micro-nano compound structure, and after processing by low-surface energy substance, surface can arrive super-hydrophobic。The method is simple to operate, reagent is cheap, effective。
It is an object of the invention to be achieved through the following technical solutions: the preparation method of a kind of aluminum surface super hydrophobic coating with micro-nano compound structure, comprise the following steps:
(1) pre-treatment: after aluminium flake is cleaned, dry in 100 DEG C of baking ovens。
(2) micron order coarse structure builds: the aluminium flake after step 1 being processed is immersed in acid etch agent and performs etching, distilled water flushing stopped reaction first used by aluminium flake after etching, it is attached to the deposit on aluminium flake again with distilled water ultrasonic cleaning, obtains the aluminum surface with micron order coarse structure。
(3) micro-nano compound coarse structure builds: being soaked in the alcoholic solution of nanoparticle by the aluminium flake after acid etch, the particle diameter of nanoparticle is 15nm 100nm, and solubility is 0.5wt% 4wt%, and soak time is 1 10min。After immersion treatment, the Muffle furnace more than 300 DEG C reacts 3 6h, obtain the aluminum surface with micro-nano compound coarse structure。
(4) low-surface energy substance processes: the resinous coat of the low-surface-energy that aluminium flake coating thickness is 0.05 0.2 μm after step 3 being processed, described resinous coat is made up of fluorine silicon resin or fluorinated silicone modified resin, then solidify 3h at 150 DEG C, super-hydrophobic coat can be obtained。
Further, described acid etch agent by hydrochloric acid, nitric acid, Fluohydric acid., sulphuric acid, oxalic acid one or more form according to any proportioning；In acid etch agent, hydrionic solubility is 1 4mol/L, and the acid etch time is 10min 16h。
Further, the temperature of described Muffle furnace is 300 600 DEG C。
Further, nanoparticle can be nano-ZnO, Nano-meter SiO_22, nanometer Fe 3O4Deng。
Further, described Nano-meter SiO_22The solubility of the alcoholic solution of particle is 0.5wt%, and soak time is 10min, Nano-meter SiO_22The particle diameter of particle is 15nm。
Further, the solubility of the alcoholic solution of described ZnO Nanoparticles is 2wt%, and soak time is 5min。The particle diameter of ZnO Nanoparticles is 50nm。
Further, described Nano-meter SiO_22The solubility of the alcoholic solution of particle is 1wt%, and particle diameter is 50nm, and soak time is 5min。
Advantages of the present invention has:
1. the present invention has prepared the Super-hydrophobic aluminium surface with micro-nano compound coarse structure, and it had both had the hydrophobicity of excellence, antifog, antifrost, deicing properties。
2. through over etching and dip-coating two-step method, going out micro-nano compound coarse structure at aluminum surface structure, method is simple to operation。
3. the raw material that the preparation of Super-hydrophobic aluminium surface is used is easy to get, and inexpensively, prepared by applicable large-area construction。
4. the super-hydrophobic aluminum flake surface prepared by the present invention, it is possible to be applied on the heat exchanger fin of air-conditioning, can effectively suppress the frosting freezing process of heat exchanger fin。
Accompanying drawing explanation
Fig. 1 is the SEM figure of the obtained product of embodiment 1；
Fig. 2 is the contact angle test figure of the obtained product of embodiment 1；
Fig. 3 is the SEM figure of the obtained product of embodiment 2；
Fig. 4 is the contact angle test figure of the obtained product of embodiment 2。
Specific embodiment
Example 1
1, aluminium flake is used respectively acetone, toluene ultrasonic cleaning 10min, then clean with distilled water, remove the greasy dirt of aluminum flake surface, dry in 100 DEG C of baking ovens。
2, clean aluminium flake is put into after the hydrochloric acid solution of 3mol/L etches 20min under room temperature, aluminium flake is taken out, clean with substantial amounts of distilled water, stopped reaction。Dry in an oven with after ultrasonic cleaning。
3, the aluminium flake obtained in step 2 is immersed in the Nano-meter SiO_2 of 15nm, 1wt%22min in alcoholic solution, reacts 3h, by Nano-meter SiO_2 in Muffle furnace at 300 DEG C after taking-up2It is grafted to aluminum surface。
4, spraying fluorinated silicone modified polyester resin on aluminium flake in step 3,150 DEG C of 3h solidify, and obtain super-hydrophobic coat。
The Super-hydrophobic aluminium surface obtained is carried out SEM scanning as it is shown in figure 1, the Nano-meter SiO_2 of the surface texture step structure by 1-2 μm and load ten a few to tens of nanometers in hierarchic structure2Structure is constituted。It is carried out contact angle test (Fig. 2) and the anti-freeze test of antifrost, and result is as shown in table 1
Example 2
1, aluminium flake is used respectively acetone, toluene ultrasonic cleaning 10min, then clean with distilled water, remove the greasy dirt of aluminum flake surface, dry in 100 DEG C of baking ovens。
2, clean aluminium flake is put into after the hydrochloric acid solution of 3mol/L etches 20min under room temperature, aluminium flake is taken out, clean with substantial amounts of distilled water, stopped reaction。Dry in an oven with after ultrasonic cleaning。
3, spraying fluorinated silicone modified polyester resin on aluminium flake in step 3,150 DEG C of 3h solidify, and obtain super-hydrophobic coat。
The Super-hydrophobic aluminium surface obtained is carried out SEM scanning as it is shown on figure 3, surface texture is made up of the step structure of 1-2 μm。It is carried out contact angle test and the anti-freeze test of antifrost。It is carried out contact angle test (Fig. 4) and the anti-freeze test of antifrost, and result is as shown in table 1
Example 3
1, aluminium flake is used respectively acetone, toluene ultrasonic cleaning 10min, then clean with distilled water, remove the greasy dirt of aluminum flake surface, dry in 100 DEG C of baking ovens。
2, clean aluminium flake is put in the hydrochloric acid of 0.5mol/L and the oxalic acid solution mixed solution of 0.5mol/L, after etching 15h under room temperature, aluminium flake is taken out, clean with substantial amounts of distilled water, stopped reaction。Dry in an oven with after ultrasonic cleaning。
3, the aluminium flake obtained in step 2 is immersed in the Nano-meter SiO_2 of 15nm, 0.5wt%210min in hexane solution, reacts 6h, by Nano-meter SiO_2 in Muffle furnace at 300 DEG C after taking-up2It is grafted to aluminum surface。
4, spraying fluorinated silicone modified polyester resin on aluminium flake in step 3,150 DEG C solidify 3h, obtain super-hydrophobic coat。
It is carried out contact angle test and the anti-freeze test of antifrost, and result is as shown in table 1。
Example 4
1, aluminium flake is used respectively acetone, toluene ultrasonic cleaning 10min, then clean with distilled water, remove the greasy dirt of aluminum flake surface, dry in 100 DEG C of baking ovens。
2, clean aluminium flake is put into after the hydrochloric acid solution of 3mol/L etches 20min under room temperature, aluminium flake is taken out, clean with substantial amounts of distilled water, stopped reaction。Dry in an oven with after ultrasonic cleaning。
3, the aluminium flake obtained in step 2 is immersed in 2min in the nano-ZnO alcoholic solution of 15nm, 2wt%, in Muffle furnace, at 500 DEG C, reacts 3h after taking-up, nano-ZnO is grafted to aluminum surface。
4, spraying fluorinated silicone modified polyester resin on aluminium flake in step 3,150 DEG C solidify 3h, obtain super-hydrophobic coat。
It is carried out contact angle test and the anti-freeze test of antifrost, and result is as shown in table 1。
Example 5
1, aluminium flake is used respectively acetone, toluene ultrasonic cleaning 10min, then clean with distilled water, remove the greasy dirt of aluminum flake surface, dry in 100 DEG C of baking ovens。
2, clean aluminium flake is put into after the hydrochloric acid of 1mol/L and the nitric acid mixed solution of 1mol/L etch 50min under room temperature, aluminium flake is taken out, clean with substantial amounts of distilled water, stopped reaction。Dry in an oven with after ultrasonic cleaning。
3, the aluminium flake obtained in step 2 is immersed in the nanometer Fe 3O of 15nm, 3wt%42min in alcoholic solution, reacts 4h, by nanometer Fe 3O in Muffle furnace at 400 DEG C after taking-up4It is grafted to aluminum surface。
4, spraying fluorinated silicone modified polyester resin on aluminium flake in step 3,150 DEG C solidify 3h, obtain super-hydrophobic coat。
It is carried out contact angle test and the anti-freeze test of antifrost, and result is as shown in table 1。
Example 6
1, aluminium flake is used respectively acetone, toluene ultrasonic cleaning 10min, then clean with distilled water, remove the greasy dirt of aluminum flake surface, dry in 100 DEG C of baking ovens。
2, clean aluminium flake is put into after the hydrochloric acid solution of 1mol/L etches 8h under room temperature, aluminium flake is taken out, clean with substantial amounts of distilled water, stopped reaction。Dry in an oven with after ultrasonic cleaning。
3, the aluminium flake obtained in step 2 is immersed in the Nano-meter SiO_2 of 50nm, 5wt%22min in alcoholic solution, reacts 3h, by Nano-meter SiO_2 in Muffle furnace at 600 DEG C after taking-up2It is grafted to aluminum surface。
4, spraying fluorinated silicone modified polyester resin on aluminium flake in step 3,150 DEG C solidify 3h, obtain super-hydrophobic coat。
It is carried out contact angle test and the anti-freeze test of antifrost, and result is as shown in table 1。
Example 7
1, aluminium flake is used respectively acetone, toluene ultrasonic cleaning 10min, then clean with distilled water, remove the greasy dirt of aluminum flake surface, dry in 100 DEG C of baking ovens。
2, clean aluminium flake is put into after the hydrochloric acid solution of 3mol/L etches 20min under room temperature, aluminium flake is taken out, clean with substantial amounts of distilled water, stopped reaction。Dry in an oven with after ultrasonic cleaning。
3, the aluminium flake obtained in step 2 is immersed in the nanometer Fe of 100nm, 3wt%3O42min in acetone soln, reacts 4h, by nanometer Fe in Muffle furnace at 400 DEG C after taking-up3O4It is grafted to aluminum surface。
4, spraying fluorinated silicone modified polyester resin on aluminium flake in step 3,150 DEG C solidify 3h, obtain super-hydrophobic coat。
It is carried out contact angle test and the anti-freeze test of antifrost, and result is as shown in table 1。
Example 8
1, aluminium flake is used respectively acetone, toluene ultrasonic cleaning 10min, then clean with distilled water, remove the greasy dirt of aluminum flake surface, dry in 100 DEG C of baking ovens。
2, clean aluminium flake is put into after the sulfuric acid solution of 2mol/L etches 40min under room temperature, aluminium flake is taken out, clean with substantial amounts of distilled water, stopped reaction。Dry in an oven with after ultrasonic cleaning。
3, the aluminium flake obtained in step 2 is immersed in the Nano-meter SiO_2 of 50nm, 1wt%22min in alcoholic solution, reacts 3h, by Nano-meter SiO_2 in Muffle furnace at 350 DEG C after taking-up2It is grafted to aluminum surface。
4, spraying fluorinated silicone modified polyester resin on aluminium flake in step 3,150 DEG C solidify 3h, obtain super-hydrophobic coat。
It is carried out contact angle test and the anti-freeze test of antifrost, and result is as shown in table 1。
The performance test data of each example of table 1
Example 9
1, aluminium flake is used respectively acetone, toluene ultrasonic cleaning 10min, then clean with distilled water, remove the greasy dirt of aluminum flake surface, dry in 100 DEG C of baking ovens。
2, clean aluminium flake is put into after the hydrochloric acid solution of 3mol/L etches 20min under room temperature, aluminium flake is taken out, clean with substantial amounts of distilled water, stopped reaction。Dry in an oven with after ultrasonic cleaning。
3, the aluminium flake obtained in step 2 is immersed in the Nano-meter SiO_2 of the 1wt% that particle diameter is 50nm20min, 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min in alcoholic solution, react 3h, by Nano-meter SiO_2 in Muffle furnace at 300 DEG C after taking-up2It is grafted to aluminum surface。
4, spraying fluorinated silicone modified polyester resin on aluminium flake in step 3,150 DEG C solidify 3h, obtain super-hydrophobic coat。
The hydrophobicity of the coating that different soak times obtain is as shown in the table:
| Soak time (min) | 0 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 |
| Static contact angle (°) | 146 | 149 | 151 | 153 | 157 | 157 | 155 | 154 | 152 |
| Roll angle (°) | 18 | 11 | 8 | 7 | 3 | 1 | 4 | 5 | 8 |
As can be seen from the table, be 1wt% particle diameter it is the SiO of 50nm when adopting concentration2During alcoholic solution, the soak time of its optimum is 5min, time is too short, owing to load nanoparticle on aluminium flake is inadequate, micro-nano compound coarse structure is inconspicuous and can not be effectively improved the hydrophobicity of coating, when overlong time is due to the excess accumulation of nanoparticle, can cover micron order coarse structure, roughness is declined on the contrary, and hydrophobic performance declines。
Claims (7)
1. the preparation method of an aluminum surface super hydrophobic coating with micro-nano compound structure, it is characterised in that comprise the following steps:
(1) pre-treatment: after aluminium flake is cleaned, dry in 100 DEG C of baking ovens。
(2) micron order coarse structure builds: the aluminium flake after step 1 being processed is immersed in acid etch agent and performs etching, distilled water flushing stopped reaction first used by aluminium flake after etching, it is attached to the deposit on aluminium flake again with distilled water ultrasonic cleaning, obtains the aluminum surface with micron order coarse structure。
(3) micro-nano compound coarse structure builds: being soaked in the alcoholic solution of nanoparticle by the aluminium flake after acid etch, the particle diameter of nanoparticle is 15nm 100nm, and solubility is 0.5wt% 4wt%, and soak time is 1 10min。After immersion treatment, the Muffle furnace more than 300 DEG C reacts 3 6h, obtain the aluminum surface with micro-nano compound coarse structure。
(4) low-surface energy substance processes: the resinous coat of the low-surface-energy that aluminium flake coating thickness is 0.05 0.2 μm after step 3 being processed, described resinous coat is made up of fluorine silicon resin or fluorinated silicone modified resin, then solidify 3h at 150 DEG C, super-hydrophobic coat can be obtained。
2. method according to claim 1, it is characterised in that described acid etch agent by hydrochloric acid, nitric acid, Fluohydric acid., sulphuric acid, oxalic acid one or more form according to any proportioning；In acid etch agent, hydrionic solubility is 1 4mol/L, and the acid etch time is 10min 16h。
3. method according to claim 1, it is characterised in that the temperature of described Muffle furnace is 300 600 DEG C。
4. method according to claim 1, it is characterised in that nanoparticle can be nano-ZnO, Nano-meter SiO_22, nanometer Fe3O4Deng。
5. method according to claim 1, it is characterised in that described Nano-meter SiO_22The solubility of the alcoholic solution of particle is 0.5wt%, and soak time is 10min, Nano-meter SiO_22The particle diameter of particle is 15nm。
6. method according to claim 1, it is characterised in that the solubility of the alcoholic solution of described ZnO Nanoparticles is 2wt%, soak time is 5min。The particle diameter of ZnO Nanoparticles is 50nm。
7. method according to claim 1, it is characterised in that described Nano-meter SiO_22The solubility of the alcoholic solution of particle is 1wt%, and particle diameter is 50nm, and soak time is 5min。
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| CN107142467B (en) * | 2017-04-25 | 2019-11-12 | 云南大学 | A kind of preparation method of super lubrication aluminium surface |
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| CN113019824A (en) * | 2021-03-23 | 2021-06-25 | 湖南大学 | Ultrasonic cavitation-based method and device for modifying surfaces of inner wall and outer wall of cavity |
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| US11851771B1 (en) | 2022-05-18 | 2023-12-26 | Guangdong University Of Technology | Method for constructing porous micro-nano structure, and material with porous micro-nano structure |
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Application publication date: 20160622 |