CN112718424A - Preparation method of frost-inhibiting and defrosting super-hydrophobic surface structure - Google Patents
Preparation method of frost-inhibiting and defrosting super-hydrophobic surface structure Download PDFInfo
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- 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
- 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
-
- 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
- B05D7/24—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 for applying particular liquids or other fluent materials
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
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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
- B05D2202/00—Metallic substrate
- B05D2202/40—Metallic substrate based on other transition elements
- B05D2202/45—Metallic substrate based on other transition elements based on Cu
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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
- B05D2518/00—Other type of polymers
- B05D2518/10—Silicon-containing polymers
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Abstract
The invention relates to a preparation method of a super-hydrophobic surface structure for frost inhibition and defrosting, which is characterized in that a micron-scale arc groove array with equal spacing moment is processed on the surface of a smooth substrate sample, the sample with the micron-scale arc groove array is cleaned and then is heated and oxidized in mixed alkali liquor, a micro-nano-scale blade-shaped structure is formed on the surface of the sample, the surface of the sample with a micro-nano topological structure is obtained, and then silanization is carried out on the surface of the sample, so that a single-molecule hydrophobic group is formed and is in a super-hydrophobic state. Compared with the prior frost prevention and defrosting technology, the invention is mainly modified by two items: firstly, directly processing a micro-nano topological structure on the surface of a metal substrate without an ultra-clean room and photoetching equipment; secondly, the surface design has the performance of frost inhibition and defrosting at the same time, the application range is wide, and the invention is suitable for heat exchangers such as various types of tube fins, microchannels and the like which take copper, aluminum or aluminum alloy as a base material.
Description
Technical Field
The invention relates to the technical field of processing and preparation, in particular to a preparation method of a frost-inhibiting and defrosting super-hydrophobic surface structure.
Background
Condensation and frost formation are the most common icing forms in industrial production, however, accumulation of frost layers often causes harm to corresponding industrial processes, and particularly, heat exchange processes of heat exchangers running under low-temperature working conditions are often seriously hindered due to thermal resistance introduced by porous structures of the frost layers.
The conventional technical means for solving the problem of the frost layer accumulation mainly include the following three types: (1) spraying alcohol organic solvent or salt to lower the freezing point of the mixed frost layer; (2) directly or indirectly absorbing external heat source to melt the frost layer, such as external infrared radiation source and embedded conductive coil; (3) and editing a cycle period of the system, such as a heat pump heating interval to perform refrigeration cycle, so that the outer machine absorbs heat to melt the attached frost layer.
The frost-inhibiting and defrosting measures usually consume a large amount of energy, influence the operation of equipment and even pollute the environment. In recent years, with the development of micro-nano processing technology represented by laser etching, a topological structure unit with a micro-nano scale is processed on the outer layer of a working surface through surface design, so that the whole device has self-cleaning capability, and the problem of frost layer accumulation can be effectively solved.
However, such processing methods rely on clean room environments and the investment of large equipment such as lithography machines, which are economically expensive and cannot be processed in large scale batches.
Disclosure of Invention
The invention aims to provide a preparation method of a frost-inhibiting and defrosting super-hydrophobic surface structure for solving the problem of frost layer accumulation.
The purpose of the invention can be realized by the following technical scheme:
a method for preparing a super-hydrophobic surface structure for inhibiting frost and defrosting comprises the steps of processing a micron-scale arc groove array with equal spacing moments on the surface of a smooth substrate sample, cleaning the sample with the micron-scale arc groove array, heating and oxidizing the sample in mixed alkali liquor to form a micro-nano-scale blade-shaped structure on the surface of the sample to obtain the surface of the sample with a micro-nano topological structure, and silanizing the surface of the sample to form a monomolecular hydrophobic group which is in a super-hydrophobic state.
Preferably, the substrate is a metal sheet, and the surface of the substrate is polished, and further preferably, the substrate is a copper sheet, an aluminum sheet or an aluminum alloy sheet, and the thickness of the substrate is 1-5 mm.
Preferably, the radian of the arc groove is 30-150 degrees, the arc length is 50-500 μm, and further preferably, the radian of the arc groove is 120 degrees, and the arc length is 500 μm.
Preferably, the micron arc groove array is processed by a micro-machining method.
Preferably, the specific method for cleaning the sample comprises the steps of soaking the sample with the micron-sized circular arc groove array in an acetone solution, cleaning the sample with ultrasonic waves, removing organic pollutants on the surface, wherein the ultrasonic wave cleaning time is at least 10 minutes, the temperature of the acetone solution is room temperature, and after the ultrasonic wave cleaning is finished, washing the surface of the sample with isopropanol and deionized water in sequence until the residual acetone solution is removed completely, and drying the sample with nitrogen.
Preferably, the mixed alkali liquor is NaClO2、NaOH、Na3PO4·12H2And (3) taking out the sample after a layer of nanoscale blade-shaped structure is formed on the surface of the sample by using the mixed solution of O and deionized water, washing the sample by using deionized water, and drying the sample by using pure nitrogen to obtain the surface of the sample with the micro-nano topological structure.
Preferably, NaClO is contained in the mixed alkali liquor2，NaOH，Na3PO4·12H2The mass ratio of O to deionized water is 3.75:5:10:100, the heating temperature is controlled to be 96 +/-3 ℃, and the heating time is 25-35 minutes.
Preferably, the silanization is carried out by a vapor phase chemical deposition method or a direct liquid phase immersion method, and when the vapor phase chemical deposition method is adopted, the sample is subjected to plasma pretreatment for not less than 1 hour. The silanized silane reagent adopts perfluoro octyl trichlorosilane, a sample with a micro-nano topological structure is placed in a vacuum tank, liquid perfluoro octyl trichlorosilane is placed on tin foil, a vacuum pump is used for vacuumizing the vacuum tank in the vacuum tank, the pressure in the vacuum tank is maintained at 10kpa, the sample is maintained for 30 minutes, and a stable super-hydrophobic coating is formed.
As a specific embodiment of the present invention, a frost and frost suppressing superhydrophobic surface structure and a method for preparing the same, includes the steps of:
processing a micron-sized arc groove array with equal moment on the surface of a sample by using a smooth copper sheet as a substrate material and adopting a micro-machining method; soaking a sample with a micron-sized circular arc groove array in an acetone solution and cleaning by using ultrasonic waves to remove organic pollutants on the surface of the sample; the sample after the completion of the washing was placed in NaClO2、NaOH、Na3PO4·12H2Heating and oxidizing in a mixed alkali liquor of O and deionized water to form a layer of nanoscale blade-shaped structure on the surface of the sample, then taking out the sample, washing the sample with deionized water, and drying with pure nitrogen to obtain the surface of the sample with a micro-nano topological structure; the surface of a sample with a micro-nano topological structure is silanized (the silanization can be completed by a gas-phase chemical deposition method or a direct liquid-phase immersion method, and a silane reagent selects perfluorooctyl trichlorosilane), and a layer of monomolecular hydrophobic groups is formed on the surface of the sample after the step, so that the sample is in a super-hydrophobic state.
The specific principle of the invention is that the frost inhibiting and defrosting mechanism of the invention utilizes the topological structure of the microgrooves and the nanometer blades to realize the spatial dimension mismatching of condensed liquid drops and block the formation of ice bridges, thereby reducing the coverage rate of a frost layer and promoting the defrosting process, wherein the arc groove structure with micron scale ensures that the local vapor pressure gradient at the groove peak position is larger than that at the groove valley position, and the liquid drops will be condensed and grow at the groove peak position firstly; and the nano blade-shaped structure with extremely low compaction rate can drive the liquid drops to generate a 'spontaneous bounce' phenomenon, so that the average size of the liquid drops at the trough is further reduced.
Therefore, the larger droplets at the trough peaks will form larger ice crystals under super-cooled conditions and will continuously absorb the water vapor volatilized from the surrounding droplets. When the smaller liquid drops at the trough can not provide the water vapor needed by the ice bridge connecting the liquid drops and the ice crystals, the liquid drops are gradually evaporated, reduced and even completely volatilized before freezing, so that the spreading of frost on the surface of the trough is blocked, a drying area is formed, and the aims of reducing the coverage rate of a frost layer and promoting defrosting are fulfilled.
Two main changes are made in the invention: firstly, directly processing a micro-nano topological structure on the surface of a metal substrate without an ultra-clean room and photoetching equipment; secondly, the surface design has the performance of inhibiting frost and defrosting simultaneously, and the application range is wide. The invention is suitable for heat exchangers such as various types of tube fins, microchannels and the like which take copper, aluminum or aluminum alloy as a base material. Compared with the prior art, the invention has the following beneficial effects:
1. in the condensation and frosting process, the coverage rate of a frost layer is effectively reduced;
2. in the defrosting process, the residual liquid amount on the surface can be greatly reduced, and secondary icing is avoided;
3. the passive defrosting scheme is achieved by surface modification without changing the structure of a heat exchanger or consuming additional mechanical work or heat energy;
4. the surface processing method is simple and economical, is suitable for various types of tube-fin heat exchangers, micro-channel heat exchangers and the like, can realize quantitative production, has considerable practical value and economic significance, and can be applied to occasions such as vehicle-mounted heat pumps, refrigerators, cold storages and the like.
Drawings
FIG. 1 and FIG. 2 are schematic views of the processing procedure of the super-hydrophobic surface structure for frost and frost inhibition and defrosting according to the present invention;
FIG. 3 is a schematic diagram of the principle of a frost suppressing and defrosting superhydrophobic surface structure suppressing ice bridge formation (frost layer propagation);
FIG. 4 is a schematic diagram of the effect of the frost-suppressing and defrosting superhydrophobic surface structure on reducing the coverage rate of frost in practical application;
in the figure: 1-smooth pure copper sheet; 2-a sample with a micron arc groove array; 3-acetone solution; 4-ultrasonic cleaning machine; 5-mixed alkali liquor; 6-a sample with a micro-nano secondary topological structure; 7-plasma cleaning machine; 8-an air valve; 9-a vacuum pump; 10-vacuum tank; 11-liquid perfluorooctyltrichlorosilane; 12-tinfoil; 13-condensing droplets; 14-freezing the droplets; 15-dendritic ice crystals; 16-superhydrophobic sample.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
Examples
In a block of 2mm thickness, 4X 4cm2The procedure for preparing the superhydrophobic sample 16 is shown in fig. 1 and 2.
Step (1): taking a block of 2mm thick 4X 4cm2The smooth pure copper sheet 1 is processed into an arc groove array with a central angle of 120 degrees and an arc length of 500 mu m on the surface of the mirror surface by a micro-machining method, and a sample 2 with a micron arc groove array is obtained.
Step (2): and (2) completely soaking the sample 2 with the micron-sized arc groove array processed in the step (1) in an acetone solution 3, and performing ultrasonic cleaning for 10 minutes by using an ultrasonic cleaning machine 4. Subsequently, the ultrasonically cleaned sample was rinsed clean with isopropyl alcohol (IPA), deionized water in that order, and dried with clean nitrogen gas.
And (3): soaking the sample 2 which is cleaned in the step (2) and has the micron arc groove array in NaClO at the temperature of 96 +/-3 DEG C2，NaOH，Na3PO4·12H2O, deionized water (3.75:5:10:100 wt%) in mixed alkali solution 5 for 30 minutes to obtain a layer of blade-like nanostructure; the sample 6 with the secondary topology is subsequently removed from the lye, rinsed clean with deionized water and dried with clean nitrogen.
And (4): and (4) putting the sample 6 with the secondary topological structure obtained in the step (3) into a plasma cleaning machine 7 for oxygen plasma cleaning for 2 hours. Immediately after the plasma cleaning process, the sample 6 having the secondary topology is placed in a vacuum tank 10, 4. mu.l of liquid perfluorooctyltrichlorosilane 11 is placed on a tin foil 12, and vacuum is applied by a vacuum pump 9 for 30 minutes to maintain the pressure in the vacuum tank 10 at 10 kpa. The vacuum pump 9 and the gas valve 8 were then turned off and the sample was maintained at a pressure of 10kpa for a further 30 minutes to form a stable superhydrophobic coating.
Referring to fig. 3 and 4, the principle of suppressing the formation of ice bridge (the spread of frost layer) in the description of the working principle of the present invention is schematically illustrated, and the effect of the surface on reducing the coverage of frost in practical application is also provided. The defrosting mechanism of the invention mainly utilizes the topological structure of micro-groove and nano blade to realize the spatial dimension mismatching of the condensed liquid drop 13 and block the formation of ice bridge, thereby reducing the coverage rate of frost layer and promoting the defrosting process, wherein, the arc groove structure with micron scale makes the partial vapor pressure gradient at the groove peak position larger than that at the groove valley position, and the liquid drop will be condensed and grown at the groove peak position firstly; and the nano blade-shaped structure with extremely low compaction rate can drive the liquid drops to generate a 'spontaneous bounce' phenomenon, so that the average size of the liquid drops at the trough is further reduced.
Thus, the larger frozen droplets 14 at the trough peaks will form larger dendritic ice crystals 15 under super-cooled conditions and will constantly absorb water vapor from the surrounding droplets. When the smaller condensate droplets 13 at the valleys do not provide the water vapor needed to connect the droplets to the ice bridge between the ice crystals 15, the droplets will gradually evaporate, shrink, or even evaporate completely before freezing, thereby impeding the spread of frost on the valley surfaces and creating a dry zone, thereby reducing the frost coverage and promoting defrosting.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of a frost-inhibiting and defrosting super-hydrophobic surface structure is characterized in that a micron-scale arc groove array with equal spacing moment is processed on the surface of a smooth substrate sample, the sample with the micron-scale arc groove array is cleaned and then heated and oxidized in mixed alkali liquor, a micro-nano-scale blade-shaped structure is formed on the surface of the sample, the surface of the sample with a micro-nano topological structure is obtained, and then silanization is carried out on the surface of the sample to form a monomolecular hydrophobic group which is in a super-hydrophobic state.
2. The method for preparing the super-hydrophobic surface structure for suppressing frost and removing frost according to claim 1, wherein the substrate is a metal sheet, and the surface is polished.
3. The preparation method of the frost and frost inhibiting super-hydrophobic surface structure according to claim 2, wherein the radian of the arc groove is 30-150 degrees, and the arc length is 50-500 μm.
4. The method for preparing the super-hydrophobic surface structure for inhibiting and removing frost and frost according to claim 1, wherein the micro-scale arc groove array is processed by a micro-machining method.
5. The method for preparing the super-hydrophobic surface structure for inhibiting and removing frost and frost according to claim 4, wherein the sample is cleaned by immersing the sample with the micron-sized circular arc groove array in an acetone solution and cleaning the sample by using ultrasonic waves to remove organic pollutants on the surface.
6. The preparation method of the frost and frost inhibiting and removing super-hydrophobic surface structure according to claim 5, wherein the ultrasonic cleaning time is at least 10 minutes, the temperature of the acetone solution is room temperature, and after the ultrasonic cleaning is finished, the surface of the sample is washed by isopropanol and deionized water in sequence until the residual acetone solution is removed and dried by nitrogen.
7. The frost and frost suppressing superhydrophobic surface structure of claim 1The preparation method of the structure is characterized in that the mixed alkali liquor is NaClO2、NaOH、Na3PO4·12H2And (3) taking out the sample after a layer of nanoscale blade-shaped structure is formed on the surface of the sample by using the mixed solution of O and deionized water, washing the sample by using deionized water, and drying the sample by using pure nitrogen to obtain the surface of the sample with the micro-nano topological structure.
8. The method for preparing the super-hydrophobic surface structure for suppressing and removing frost and frost according to claim 7, wherein NaClO is in the mixed alkali solution2，NaOH，Na3PO4·12H2The mass ratio of O to deionized water is 3.75:5:10:100, the heating temperature is controlled to be 96 +/-3 ℃, and the heating time is 25-35 minutes.
9. The method for preparing the super-hydrophobic surface structure for inhibiting frost and removing frost according to claim 1, wherein the silanization is performed by a vapor phase chemical deposition method or a direct liquid phase immersion method, and when the vapor phase chemical deposition method is adopted, a sample is subjected to plasma pretreatment for not less than 1 hour.
10. The method for preparing the super-hydrophobic surface structure for inhibiting frost and defrosting according to claim 9, wherein the silanized silane reagent adopts perfluorooctyl trichlorosilane, the sample with the micro-nano topological structure is placed in a vacuum tank, the liquid perfluorooctyl trichlorosilane is placed on tin foil, the vacuum tank is vacuumized by using a vacuum pump, the pressure in the vacuum tank is maintained at 10kpa, and the sample is maintained for 30 minutes to form the stable super-hydrophobic coating.
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