CN111270227A - Method for preparing micro-nano needle convex super-hydrophobic surface by utilizing microwave - Google Patents
Method for preparing micro-nano needle convex super-hydrophobic surface by utilizing microwave Download PDFInfo
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- CN111270227A CN111270227A CN202010094267.7A CN202010094267A CN111270227A CN 111270227 A CN111270227 A CN 111270227A CN 202010094267 A CN202010094267 A CN 202010094267A CN 111270227 A CN111270227 A CN 111270227A
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- 238000000034 method Methods 0.000 title claims abstract description 42
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 202
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 97
- 241000931705 Cicada Species 0.000 claims abstract description 68
- 229910052751 metal Inorganic materials 0.000 claims abstract description 65
- 239000002184 metal Substances 0.000 claims abstract description 65
- 239000000843 powder Substances 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000009713 electroplating Methods 0.000 claims description 41
- 238000007747 plating Methods 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 239000000126 substance Substances 0.000 claims description 32
- 229910001868 water Inorganic materials 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 19
- 238000004140 cleaning Methods 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 238000000151 deposition Methods 0.000 claims description 13
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 12
- 229910052737 gold Inorganic materials 0.000 claims description 12
- 239000010931 gold Substances 0.000 claims description 12
- 238000011049 filling Methods 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- 229910021205 NaH2PO2 Inorganic materials 0.000 claims description 8
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 8
- 238000003760 magnetic stirring Methods 0.000 claims description 8
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 8
- 230000001235 sensitizing effect Effects 0.000 claims description 8
- 230000004913 activation Effects 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910002666 PdCl2 Inorganic materials 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 2
- 230000008021 deposition Effects 0.000 abstract description 6
- 238000002848 electrochemical method Methods 0.000 abstract description 3
- 238000009768 microwave sintering Methods 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 42
- 240000002853 Nelumbo nucifera Species 0.000 description 15
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 15
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 15
- 239000002086 nanomaterial Substances 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 10
- 238000002310 reflectometry Methods 0.000 description 9
- 239000012620 biological material Substances 0.000 description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 7
- 241000080590 Niso Species 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000008151 electrolyte solution Substances 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 239000011664 nicotinic acid Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 101150003085 Pdcl gene Proteins 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008313 sensitization Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
Images
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1655—Process features
- C23C18/1657—Electroless forming, i.e. substrate removed or destroyed at the end of the process
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/2006—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
- C23C18/2046—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by chemical pretreatment
- C23C18/2073—Multistep pretreatment
- C23C18/2086—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1054—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by microwave
Abstract
The invention belongs to the technical field of super-hydrophobic, and particularly discloses a method for preparing a micro-nano needle convex super-hydrophobic surface by using microwaves. The surface of the cicada wing is cleaned in advance, a conductive nickel layer is chemically plated on the surface of the cicada wing, a nickel deposition layer with the thickness of 200-500 mu m is plated on the surface of the cicada wing through an electrochemical method, the cicada wing is stripped to obtain a nickel template with micro-nano pits, the nickel template is placed in a forming die and filled with superfine metal powder, the metal powder is sintered through microwave heating, and the metal surface with micro-nano needle protrusions is prepared. The invention adopts an electrochemical method to prepare the nickel replica with the conical nano-holes by taking the cicada wing as an original template. And then, performing microwave sintering molding, taking the nickel replica as a template, transcribing the conical nano holes to the surface of the metal to form ordered and dense nano columns, wherein the average diameter is 120-165 nm, and the average screw pitch is 155-220 nm. At the same time, the nickel replica produced is reusable.
Description
Technical Field
The invention belongs to the technical field of super-hydrophobic, and particularly relates to a method for preparing a micro-nano needle convex super-hydrophobic surface by using microwaves.
Background
The hydrophobicity of natural biological materials is a natural phenomenon, and in nature, many organisms have various excellent surface super-hydrophobic characteristics because almost perfect micro/nano structures exist on the surfaces of the organisms, and the artificial micro-nano structures are copied to new functional surfaces, so that the preparation of the bionic super-hydrophobic materials gradually becomes a leading-edge science along with the development of science and technology.
The preparation method of the bionic super-hydrophobic material in the prior art comprises the following steps: the existing preparation methods have the defects of needing special processing equipment and complex technological processes, having higher cost, poorer reliability and the like. In addition, the micro-nano structure on the surface of the natural biological material is very fine, and the direct deposition of metal on the surface of the natural biological material is very difficult, so that the application of the bionic micro/nano structure surface with excellent functions is limited. Therefore, a continuous and simple method needs to be provided for copying the micro-nano structure in the bionic template.
Disclosure of Invention
The invention aims to solve the technical problems pointed out in the background technology part and save cost, and provides a method for preparing a micro-nano needle convex super-hydrophobic surface by using microwaves.
The invention discloses a method for preparing a micro-nano needle convex super-hydrophobic surface by utilizing microwave, which comprises the following steps:
(1) cleaning cicada wing: washing the cicada wing with deionized water for 15-20 min, then ultrasonically cleaning with acetone for 15-20 min, then ultrasonically cleaning with deionized water for 8-10 min, removing residual acetone, and finally drying in a vacuum oven at 40 ℃.
(2) Activation treatment of cicada's wing: immersing the cicada wing dried in the step (1) into a sensitizing solution at the temperature of 22-28 ℃ for 8-13 min, and then immersing in an activating solution for 3-6 min. And naturally drying in the air to obtain the pretreated cicada wing sample.
Wherein the composition of the sensitizing solution is 10g/L SnCl2·H2O、40ml/L HCl、1g/L C12H25SO4Na；
The composition of the activation solution was 1g/L PdCl2·H2O、10ml/L HCl。
(3) Preparing a nickel template: fixing the cicada wing pretreated in the step (2) on a glass plate, then immersing the cicada wing in a chemical nickel plating solution, adjusting the pH value of the solution to 8.5 by using ammonia water, carrying out magnetic stirring at the temperature of 35-40 ℃ and the rotating speed of 145-155 r/min, chemically plating a conductive nickel layer on the surface of the cicada wing after 8-12 min of chemical plating, taking out the cicada wing from the solution, and thoroughly washing the cicada wing by using deionized water. And then, electroplating at 45-50 ℃ by taking the cicada wing covered by the conductive nickel as a cathode and the Ni-S plate as an anode. Electroplating for 100-140 min. A nickel plating layer having a thickness of 200 to 500 μm is deposited on the conductive nickel layer in the plating solution. And after cleaning and drying, peeling the cicada wing from the nickel layer to obtain the nickel template with the micro-nano pits.
Wherein the chemical nickel plating solution comprises 30g/L NiSO4·6H2O、30g/L NaH2PO2·H2O、20g/L Na3C6H5O7·2H2O；
The composition of the electroplating solution in the electroplating process is 300g/L Ni (SO)3NH2)2·4H2O、15g/L NiCl2·6H2O、20g/L H3BO3。
The constant current density is 3-4A/dm during nickel electroplating2。
According to the method, the template is prepared by depositing metal through chemical plating and electroplating, a thin and uniform conducting layer can be obtained through chemical plating, a deposited layer with a certain thickness can be obtained through electroplating, and the prepared template has good reusability.
(4) Preparing a convex surface of the metal micro-nano needle: and (4) taking the nickel template with the micro-nano pits prepared in the step (3) as a template, filling superfine metal powder subjected to ball milling by a ball mill on the template, filling the metal powder on the surface of the template, paving a metal powder layer with the thickness of 200-500 mu m, and compacting. Under the microwave heating condition, heating the template filled with the metal powder to about 1200 ℃, preserving the heat for 1h, cooling and removing the nickel template to obtain the metal surface with the micro-nano needle protrusions.
Wherein, the metal powder is one or more of gold, silver, copper, aluminum or zinc.
The particle size of the metal powder is 300-500 meshes.
The microwave frequency is 300 MHz-30 GHz, and the output power of the microwave source is 0.3-2.6 kW.
The average diameter of ordered and dense nano columns formed by the micro-nano needle convex structure on the surface of the prepared micro-nano needle convex metal is 120-165 nm, and the average thread pitch is 155-220 nm.
The invention has the beneficial effects that:
1. the ordered and densely arranged metal micro-nano structures are prepared by adopting a process combining an electrochemical method and a microwave sintering method, and show the super-hydrophobic characteristics inherited from cicada wings.
2. The nickel template in the preparation method has reusability, and avoids the characteristics of complicated operation method, high preparation cost, poor durability and the like in the existing super-hydrophobic preparation technology.
Drawings
Fig. 1 is a scanning electron microscope image of the nano-structure on the surface of the cicada wing and the lotus leaf, wherein, (a) the cicada wing and (b) the lotus leaf.
FIG. 2 is a specific process schematic diagram of the preparation of the micro-nano needle convex super-hydrophobic surface.
Fig. 3 is a scanning electron microscope image of the micro-nano surface prepared in example 1.
FIG. 4 is a scanning electron micrograph of the nickel template prepared in example 1.
Fig. 5 is a scanning electron microscope image of the micro-nano surface prepared in example 2.
FIG. 6 is a bar graph of water contact angles for examples 1, 2, 3, 4 and comparative examples 1, 2, 3, 4.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1
Step 1, washing the cicada wing with deionized water for 20min, then ultrasonically cleaning the cicada wing with acetone for 20min, finally ultrasonically cleaning the cicada wing with deionized water for 10min, removing residual acetone, and then drying the cicada wing in a vacuum oven at 40 ℃.
Step 2, the cicada's wing cleaned and dried in the step 1 is firstly put in a sensitizing solution (the composition of the sensitizing solution is 10g/L SnCl) at 25 DEG C2·H2O、40ml/L HCl、1g/L C12H25SO4Na) for 10min, and then in an activation solution (the composition of the activation solution is 1g/L PdCl) at 25 DEG C2·H2O, 10ml/L HCl) for 5 min. During sensitization, sodium dodecyl sulfate (C)12H25SO4Na) as a surfactant to improve hydrogenation performance. And then, naturally drying the cicada wing in the air to obtain the pretreated cicada wing.
Step 3, fixing the natural cicada wing pretreated in the step 2 on supporting glass by adopting chemical plating, and then immersing the natural cicada wing in chemical nickel plating solution (the chemical nickel plating solution comprises 30g/L NiSO)4·6H2O、30g/L NaH2PO2·H2O、20g/LNa3C6H5O7·2H2O), adjusting the pH value of the solution to 8.5 by ammonia water, and magnetically stirring at 40 ℃ and the rotating speed of 150 r/min. And depositing a conductive nickel layer on the surface of the natural cicada wing by the chemical plating. Subsequently, the conductive nickel-coated cicada' S wing was used as a cathode and a Ni-S plate was used as an anode, and electroplating was performed at 50 ℃ (composition of electroplating solution was 300g/L Ni (SO)3NH2)2·4H2O、15g/L NiCl2·6H2O、20g/L H3BO3) Constant current density of 4A/dm2. In order to ensure the uniformity of the electrolyte solution, the magnetic stirring is carried out at a rotating speed of 150 r/min. After 120min of electroplating, a nickel deposition layer having a thickness of about 400 μm was deposited on the conductive nickel layer in the electroplating bath. After cleaning and drying, the nickel layer is stripped from the cicada's wing to obtain a replica of nickel.
And 4, taking the nickel replica prepared in the step 3 as a template, filling superfine metal powder (the gold particle size is 300 meshes) subjected to ball milling by a ball mill on the surface of the template, and compacting. Under the microwave heating condition, heating the template filled with the metal powder to 1200 ℃, preserving the heat for 1h, wherein the microwave frequency is 12.5GHz, the output power of a microwave source is 1.5kW, and removing the nickel template after cooling to obtain the gold metal surface with the micro-nano needle protrusions.
The average diameter of the micro-nano needle convex structure on the metal replica prepared by the steps is about 156nm, and the average thread pitch is about 180 nm. The water contact angle of the surface of the metal replica in the wavelength range of 400-1000nm is 163 +/-2 degrees, and the reflectivity is about 6 percent. Thus, the hydrophobicity and reflectivity of natural cicada wings are inherited by the metal replica.
Example 2
Step 1, step 2 and step 3, the same as in example 1.
And 4, taking the nickel replica prepared in the step 3 as a template, filling superfine metal powder (the zinc particle size is 300 meshes) subjected to ball milling by a ball mill on the surface of the template, and compacting. Under the microwave heating condition, heating the template filled with the metal powder to 1200 ℃, preserving the heat for 1h, wherein the microwave frequency is 10.5GHz, the output power of a microwave source is 2kW, and removing the nickel template after cooling to obtain the zinc metal surface with the micro-nano needle protrusions.
The average diameter of the micro-nano needle convex structure on the metal replica prepared by the steps is about 152nm, and the average thread pitch is about 220 nm. The water contact angle of the surface of the metal replica in the wavelength range of 400-1000nm is 158 degrees +/-2 degrees, and the reflectivity is about 4 percent.
Example 3
Step 1 and step 2, the same as in example 1.
Step 3, fixing the natural cicada wing pretreated in the step 2 on supporting glass by adopting chemical plating, and then immersing the natural cicada wing in chemical nickel plating solution (the chemical nickel plating solution comprises 30g/L NiSO)4·6H2O、30g/L NaH2PO2·H2O、20g/LNa3C6H5O7·2H2O), adjusting the pH value of the solution to 8.5 by ammonia water, and magnetically stirring at 40 ℃ and the rotating speed of 150 r/min. And depositing a conductive nickel layer on the surface of the natural cicada wing by the chemical plating. Subsequently, the conductive nickel-coated cicada' S wing was used as a cathode and a Ni-S plate was used as an anode, and electroplating was performed at 50 ℃ (composition of electroplating solution was 300g/L Ni (SO)3NH2)2·4H2O、15g/L NiCl2·6H2O、20g/L H3BO3) Constant current density of 3A/dm2. To ensure the electrolyte solutionThe uniformity of the mixture is realized by adopting magnetic stirring at the rotating speed of 150 r/min. After 120min of electroplating, a nickel deposition layer having a thickness of about 300 μm was deposited on the conductive nickel layer in the electroplating bath. After cleaning and drying, the nickel layer is stripped from the cicada's wing to obtain a replica of nickel.
And 4, taking the nickel replica prepared in the step 3 as a template, filling superfine metal powder (the gold particle size is 300 meshes) subjected to ball milling by a ball mill on the surface of the template, and compacting. Under the microwave heating condition, heating the template filled with the metal powder to 1200 ℃, preserving the heat for 1h, wherein the microwave frequency is 12.5GHz, the output power of a microwave source is 1.5kW, and removing the nickel template after cooling to obtain the gold metal surface with the micro-nano needle protrusions.
The average diameter of the micro-nano needle convex structure on the metal replica prepared by the steps is about 121nm, and the average thread pitch is about 210 nm. The water contact angle of the surface of the metal replica in the wavelength range of 400-1000nm is 152 DEG +/-2 DEG, and the reflectivity is about 3%.
Example 4
Step 1 and step 2, the same as in example 1.
Step 3, fixing the natural cicada wing pretreated in the step 2 on supporting glass by adopting chemical plating, and then immersing the natural cicada wing in chemical nickel plating solution (the chemical nickel plating solution comprises 30g/L NiSO)4·6H2O、30g/L NaH2PO2·H2O、20g/LNa3C6H5O7·2H2O), adjusting the pH value of the solution to 8.5 by ammonia water, and magnetically stirring at 40 ℃ and the rotating speed of 150 r/min. And depositing a conductive nickel layer on the surface of the natural cicada wing by the chemical plating. Subsequently, the conductive nickel-coated cicada' S wing was used as a cathode and a Ni-S plate was used as an anode, and electroplating was performed at 50 ℃ (composition of electroplating solution was 300g/L Ni (SO)3NH2)2·4H2O、15g/L NiCl2·6H2O、20g/L H3BO3) Constant current density of 4A/dm2. In order to ensure the uniformity of the electrolyte solution, the magnetic stirring is carried out at a rotating speed of 150 r/min. After 140min of electroplating, a nickel deposit layer having a thickness of about 480 μm was deposited on the conductive nickel layer in the electroplating bath. After cleaning and drying, the nickel layer is stripped from the cicada's wing to obtain a replica of nickel.
And 4, taking the nickel replica prepared in the step 3 as a template, filling superfine metal powder (the gold particle size is 300 meshes) subjected to ball milling by a ball mill on the surface of the template, and compacting. Under the microwave heating condition, heating the template filled with the metal powder to 1200 ℃, preserving the heat for 1h, wherein the microwave frequency is 12.5GHz, the output power of a microwave source is 1.5kW, and removing the nickel template after cooling to obtain the gold metal surface with the micro-nano needle protrusions.
The average diameter of the micro-nano needle convex structure on the metal replica prepared by the steps is about 165nm, and the average thread pitch is about 155 nm. The water contact angle of the surface of the metal replica in the wavelength range of 400-1000nm is 150 +/-2 degrees, and the reflectivity is about 3 percent.
Comparative example 1
The method is characterized in that a natural biological material, namely lotus leaves, is used as a template, and a hydrophobic metal surface which has hydrophobicity and is consistent with the micro texture of the surface of a biological prototype is prepared by combining an electroplating process and a microwave process, and comprises the following steps:
step 1, washing lotus leaves with deionized water for 20min, then ultrasonically cleaning the lotus leaves with acetone for 20min, finally ultrasonically cleaning the lotus leaves with deionized water for 10min, removing residual acetone, and then drying the lotus leaves in a vacuum oven at 40 ℃.
Step 2, the lotus leaves cleaned and dried in the step 1 are firstly put in a sensitizing solution (the composition of the sensitizing solution is 10g/L SnCl) at the temperature of 25 DEG C2·H2O、40ml/L HCl、1g/L C12H25SO4Na) for 10min, and then in an activation solution (the composition of the activation solution is 1g/L PdCl) at 25 DEG C2·H2O, 10ml/L HCl) for 5 min. During sensitization, sodium dodecyl sulfate (C)12H25SO4Na) as a surfactant to improve hydrogenation performance. Then, the lotus leaves are naturally dried in the air, and the pretreated lotus leaves are obtained.
Step 3, fixing the pretreated natural lotus leaves on supporting glass by adopting chemical plating, and then immersing the natural lotus leaves in chemical nickel plating solution (the chemical nickel plating solution comprises 30g/L NiSO)4·6H2O、30g/L NaH2PO2·H2O、20g/LNa3C6H5O7·2H2O), magnetically stirring at 40 ℃ and 150 r/min. The pH of the solution was adjusted to 8.5 with aqueous ammonia. And depositing a conductive nickel layer on the surface of the natural lotus leaf by the chemical plating. Subsequently, the lotus leaves covered with conductive nickel were used as a cathode, and a Ni-S plate was used as an anode, and electroplating was carried out at 50 ℃ (the composition of the electroplating solution was 300g/L Ni (SO)3NH2)2·4H2O、15g/L NiCl2·6H2O、20g/L H3BO3) Constant current density of 4A/dm2. In order to ensure the uniformity of the electrolyte solution, the magnetic stirring is carried out at a rotating speed of 150 r/min. After 120min of electroplating, a nickel deposition layer having a thickness of about 400 μm was deposited on the conductive nickel layer in the electroplating bath. After cleaning and drying, the nickel layer is stripped from the lotus leaves to obtain a replica of nickel.
And 4, taking the nickel replica prepared in the step 3 as a template, filling superfine metal powder (the gold particle size is 300 meshes) subjected to ball milling by a ball mill on the surface of the template, and compacting. Under the microwave heating condition, heating the template filled with the metal powder to 1200 ℃, preserving the heat for 1h, wherein the microwave frequency is 12.5GHz, the output power of a microwave source is 1.5kW, and removing the nickel template after cooling to obtain the metal surface with the micro-nano structure.
The average diameter of the micro-microprotrusion structure on the metal replica prepared by the above steps is about 200nm, and the average thread pitch is about 20 μm. The water contact angle of the surface of the metal replica in the wavelength range of 400-1000nm is 138 +/-2 degrees, and the reflectivity is about 1 percent.
Comparative example 2
The preparation method is characterized in that cicada's wing made of natural biological materials is used as a template, and a hydrophobic metal surface which has hydrophobicity and is consistent with the micro-texture of the surface of a biological prototype is prepared by combining an electroplating process and a normal-pressure sintering process, and the method comprises the following steps:
step 1, step 2 and step 3, the same as in example 1.
And 4, taking the nickel replica prepared previously as a template, filling superfine metal powder (the gold particle size is 300 meshes) subjected to ball milling by a ball mill on the surface of the template, and compacting. And (3) placing the mixture into an ITO normal pressure sintering furnace, preserving heat for 1h under the high temperature condition (about 900-.
The average diameter of the micro-nano needle convex structure on the metal replica prepared by the steps is about 250nm, and the average thread pitch is about 10 mu m. The water contact angle of the surface of the metal replica in the wavelength range of 400-1000nm is 126 +/-2 degrees, and the reflectivity is about 2 percent.
Comparative example 3
The preparation method is characterized in that cicada's wing made of natural biological materials is used as a template, and a hydrophobic metal surface which has hydrophobicity and is consistent with the micro texture of the surface of a biological prototype is prepared by combining an electroplating process and a microwave process, and the method comprises the following steps:
step 1 and step 2, the same as in example 1.
Step 3, fixing the natural cicada wing pretreated in the step 2 on supporting glass by adopting chemical plating, and then immersing the natural cicada wing in chemical nickel plating solution (the chemical nickel plating solution comprises 30g/L NiSO)4·6H2O、30g/L NaH2PO2·H2O、20g/LNa3C6H5O7·2H2O), magnetically stirring at 40 ℃ and 150 r/min. The pH of the solution was adjusted to 8.5 with aqueous ammonia. And depositing a conductive nickel layer on the surface of the natural cicada wing by the chemical plating. Subsequently, the conductive nickel-coated cicada' S wing was used as a cathode and a Ni-S plate was used as an anode, and electroplating was performed at 50 ℃ (composition of electroplating solution was 300g/L Ni (SO)3NH2)2·4H2O、15g/L NiCl2·6H2O、20g/L H3BO3) Constant current density of 4A/dm2. In order to ensure the uniformity of the electrolyte solution, the magnetic stirring is carried out at a rotating speed of 150 r/min. After 200min of electroplating, a nickel deposit layer having a thickness of about 580 μm was deposited on the conductive nickel layer in the electroplating bath. After cleaning and drying, the nickel layer is stripped from the cicada's wing to obtain a replica of nickel.
And 4, taking the nickel replica prepared in the step 3 as a template, filling superfine metal powder (the gold particle size is 300 meshes) subjected to ball milling by a ball mill on the surface of the template, and compacting. Under the microwave heating condition, heating the template filled with the metal powder to 1200 ℃, preserving the heat for 1h, wherein the microwave frequency is 12.5GHz, the output power of a microwave source is 1.5kW, and removing the nickel template after cooling to obtain the metal surface with the micro-nano structure.
The average diameter of the micro-nano needle convex structure on the prepared metal replica is about 200nm, and the average thread pitch is about 20 mu m. The water contact angle of the surface of the metal replica in the wavelength range of 400-1000nm is 101 +/-2 degrees, and the reflectivity is about 1 percent.
Comparative example 4
The preparation method is characterized in that cicada's wing made of natural biological materials is used as a template, and a hydrophobic metal surface which has hydrophobicity and is consistent with the micro texture of the surface of a biological prototype is prepared by combining an electroplating process and a microwave process, and the method comprises the following steps:
step 1 and step 2, the same as in example 1.
Step 3, fixing the natural cicada wing pretreated in the step 2 on supporting glass by adopting chemical plating, and then immersing the natural cicada wing in chemical nickel plating solution (the chemical nickel plating solution comprises 30g/L NiSO)4·6H2O、30g/L NaH2PO2·H2O、20g/LNa3C6H5O7·2H2O), magnetically stirring at 40 ℃ and 150 r/min. The pH of the solution was adjusted to 8.5 with aqueous ammonia. And depositing a conductive nickel layer on the surface of the natural cicada wing by the chemical plating. Subsequently, the conductive nickel-coated cicada' S wing was used as a cathode and a Ni-S plate was used as an anode, and electroplating was performed at 50 ℃ (composition of electroplating solution was 300g/L Ni (SO)3NH2)2·4H2O、15g/L NiCl2·6H2O、20g/L H3BO3) Constant current density of 5A/dm2. In order to ensure the uniformity of the electrolyte solution, the magnetic stirring is carried out at a rotating speed of 150 r/min. After 120min of electroplating, a nickel deposition layer with a thickness of about 600 μm was deposited on the conductive nickel layer in the electroplating bath. After cleaning and drying, the nickel layer is stripped from the cicada's wing to obtain a replica of nickel.
And 4, taking the nickel replica prepared in the step 3 as a template, filling superfine metal powder (the gold particle size is 300 meshes) subjected to ball milling by a ball mill on the surface of the template, and compacting. Under the microwave heating condition, heating the template filled with the metal powder to 1200 ℃, preserving the heat for 1h, wherein the microwave frequency is 12.5GHz, the output power of a microwave source is 1.5kW, and removing the nickel template after cooling to obtain the metal surface with the micro-nano structure.
The average diameter of the micro-nano needle convex structure on the prepared metal replica is about 270nm, and the average thread pitch is about 12 mu m. The water contact angle of the surface of the metal replica in the wavelength range of 400-1000nm is 115 +/-2 degrees, and the reflectivity is about 1 percent.
Claims (9)
1. A method for preparing a micro-nano needle convex super-hydrophobic surface by using microwaves is characterized by comprising the following specific steps:
(1) cleaning cicada wing: washing the cicada wing with deionized water for 15-20 min, then ultrasonically cleaning with acetone for 15-20 min, then ultrasonically cleaning with deionized water for 8-10 min, removing residual acetone, and finally drying in a vacuum oven at 40 ℃;
(2) activation treatment of cicada's wing: immersing the cicada wing dried in the step (1) into a sensitizing solution at 22-28 ℃ for 8-13 min, then immersing in an activating solution for 3-6 min, and naturally drying in the air to obtain a pretreated cicada wing sample;
(3) preparing a nickel template: fixing the cicada wing pretreated in the step (2) on a glass plate, then immersing the cicada wing in a chemical nickel plating solution, adjusting the pH value of the solution to 8.5 by using ammonia water, carrying out magnetic stirring chemical nickel plating for 8-12 min at the temperature of 35-40 ℃ and the rotating speed of 145-155 r/min, then chemically plating a conductive nickel layer on the surface of the cicada wing, taking out the cicada wing from the solution, and thoroughly washing the cicada wing by using deionized water; then, electroplating at 45-50 ℃ by taking the cicada wing covered by the conductive nickel as a cathode and the Ni-S plate as an anode, depositing a nickel plating layer with the thickness of 200-500 mu m on the conductive nickel layer in the electroplating solution after electroplating for 100-140 min, and stripping the cicada wing from the nickel plating layer after cleaning and drying to obtain a nickel template with micro-nano pits;
(4) preparing a convex surface of the metal micro-nano needle: filling superfine metal powder subjected to ball milling by a ball mill on the nickel template with the micro-nano pits prepared in the step (3) as a template, and compacting; under the microwave heating condition, heating the template filled with the metal powder to about 1200 ℃, preserving the heat for 1h, cooling and removing the nickel template to obtain the metal surface with the micro-nano needle protrusions.
2. The method for preparing the micro-nano needle convex superhydrophobic surface by using the microwave according to claim 1: the method is characterized in that: the composition of the sensitizing solution in the step (2) is 10g/L SnCl2·H2O、40ml/L HCl、1g/L C12H25SO4Na。
3. The method for preparing the micro-nano needle convex superhydrophobic surface by using the microwave according to claim 1: the method is characterized in that: the composition of the activating solution in the step (2) is 1g/L PdCl2·H2O、10ml/L HCl。
4. The method for preparing the micro-nano needle convex superhydrophobic surface by using the microwave according to claim 1: the method is characterized in that: the chemical nickel plating solution in the step (3) has the composition of 30g/L NiSO4·6H2O、30g/L NaH2PO2·H2O、20g/LNa3C6H5O7.2H2O。
5. The method for preparing the micro-nano needle convex superhydrophobic surface by using the microwave according to claim 1: the method is characterized in that: the composition of the electroplating solution adopted in the electroplating in the step (3) is 300g/L of Ni (SO)3NH2)2·4H2O、15g/L NiCl2·6H2O、20g/LH3BO3。
6. The method for preparing the micro-nano needle convex superhydrophobic surface by using the microwave according to claim 1: the method is characterized in that: the constant current density is 3-4A/dm during the nickel electroplating in the step (3)2。
7. The method for preparing the micro-nano needle convex superhydrophobic surface by using the microwave according to claim 1: the method is characterized in that: the metal powder in the step (4) is one or more of gold, silver, copper, aluminum or zinc; the metal powder has a particle size of 300 to 500 mesh.
8. The method for preparing the micro-nano needle convex superhydrophobic surface by using the microwave according to claim 1: the method is characterized in that: in the step (4), the microwave frequency is 300 MHz-30 GHz, and the output power of the microwave source is 0.3-2.6 kW.
9. A micro-nano needle convex superhydrophobic surface prepared according to the method of claim 1.
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