CN106367739A - Method for preparing brass-based super-hydrophobic microstructural surface - Google Patents

Method for preparing brass-based super-hydrophobic microstructural surface Download PDF

Info

Publication number
CN106367739A
CN106367739A CN201611094585.3A CN201611094585A CN106367739A CN 106367739 A CN106367739 A CN 106367739A CN 201611094585 A CN201611094585 A CN 201611094585A CN 106367739 A CN106367739 A CN 106367739A
Authority
CN
China
Prior art keywords
sample
laser
preparation
super hydrophobic
based super
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201611094585.3A
Other languages
Chinese (zh)
Inventor
叶霞
黄超
姚爱斐
杨晓红
范振敏
刘群超
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu University of Technology
Original Assignee
Jiangsu University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu University of Technology filed Critical Jiangsu University of Technology
Priority to CN201611094585.3A priority Critical patent/CN106367739A/en
Publication of CN106367739A publication Critical patent/CN106367739A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical 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
    • C23C22/02Chemical 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 non-aqueous solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B41PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41JTYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
    • B41J2/00Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
    • B41J2/435Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by selective application of radiation to a printing material or impression-transfer material
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/02Chemical 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 thermal decomposition
    • C23C18/12Chemical 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 thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204Chemical 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 thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208Oxides, e.g. ceramics
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/02Chemical 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 thermal decomposition
    • C23C18/12Chemical 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 thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1229Composition of the substrate
    • C23C18/1241Metallic substrates
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/02Chemical 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 thermal decomposition
    • C23C18/12Chemical 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 thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125Process of deposition of the inorganic material
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical 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
    • C23C22/78Pretreatment of the material to be coated
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C2222/00Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
    • C23C2222/20Use of solutions containing silanes

Abstract

The invention belongs to the technical field of metal-based microstructural surface design preparation and laser micro-processing, and discloses a method for preparing a brass-based super-hydrophobic microstructural surface. The method comprises the following steps: (1) performing pretreatment, namely, grinding a brass sample, washing, and drying so as to obtain the brass sample; (2) performing laser micro-processing, namely, performing laser scanning treatment on the surface of the sample by using an infrared laser labeling machine; (3) performing hydrothermal treatment, namely, washing the sample after laser micro-processing so as to remove flying spray, putting the sample and a zinc sheet into mixed liquid of distilled water and formamide, and performing hydro-thermal treatment inside a hydro-thermal reaction kettle; and (4) performing surface modification, namely, soaking the sample after hydro-thermal treatment into an ethanol solution of 1H,1H,2H,2H-perfluorodecyl triethoxysilane to form a layer of a hydrophobic membrane on the surface of the sample, taking out the sample, and drying, thereby obtaining the super-hydrophobic surface. According to the method, the preparation process is simple, and the brass-based super-hydrophobic microstructural surface can be prepared in an atmospheric environment.

Description

A kind of preparation method of pyrite based super hydrophobic micro-structure surface
Technical field
The invention belongs to the design preparation of Metal Substrate micro-structure surface and laser micro-machining technology field, refer in particular to preparation condition It is designed, and prepare the side of pyrite based super hydrophobic micro-structure surface using the technology that Laser Micro-Machining and hydrothermal treatment consists combine Method.
Background technology
Pyrite as a kind of important engineering metal material, because its have good mechanical property, thermoplasticity, machinability, Easily welding, electrical and thermal conductivity be good, low price the features such as, be commonly used for manufacturing condenser, water pipe, air-conditioning connection pipe for internal-external unit, The parts such as radiator, pin, conduit.But the surface energy of copper is higher, the moisture of easily absorption in the air causes corrosion failure, impact The serviceability of product and service life.
The eighties in 20th century, botanist barthlott and neihuis of Univ Bonn Germany is by tying to lotus leaf surface The observation of structure finds the raised and wax-like organizational structure of micron order that its surface exists so that Folium Nelumbinis have super-hydrophobicity (i.e. water It is dropped in leaf surfaces and can automatically be gathered into the globule and be rolled down) cause worldwide very big concern.It has been investigated that Super hydrophobic surface has plurality of advantages, if super hydrophobic surface is acted on can play automatically cleaning, anticorrosive, sliding on metal material Move drag reduction, reduce friction, strengthen absorbance of light and other effects.Such as super hydrophobic surface is used in petroleum transportation pipeline, can prevent Duct wall viscous reduces loss and energy expenditure in transportation;Super hydrophobic surface is used for optical instrument, sensor and too In the parts such as sun energy conversion equipment, the reflection to light can be efficiently reduced, absorb incident illumination to greatest extent;Super hydrophobic material is used In industries such as boat oceangoing ships, such as apply last layer based superhydrophobic thin films in hull, the friction with water in ship traveling process can be substantially reduced, section Save fuel oil;Super hydrophobic material is used for bio-medical tissue such as the body structure surface such as artificial blood vessel, intravascular stent, Cardiac valve prosthesiss On, the blood compatibility of biology can be improved, reduce thrombotic probability.Therefore act on brass surfaces with laser marking machine, Prepare the micro-structure surface with super-hydrophobicity, corrosion resistance, the rub of material can be improved.
The preparation method of metal current based super hydrophobic function surface mainly has chemical etching method, anodizing, gas phase to sink Area method, laser ablation method etc.., because of its wide adaptability, crudy is stable, processing dimension is controlled and is subject to people for laser etching techniques Extensive concern.Patent as Application No. 200810019368.7 discloses a kind of metal base ultra-hydrophobicity micro-structure surface Laser preparation method, Metal Substrate micro structure table is prepared by femtosecond laser under vacuum environment using oxidizing process or method with plastic film Face, can realize the super-hydrophobicity of material surface in the case of without any surface treatment.Application No. 200910021923.4 Patent disclose a kind of method that femtosecond laser prepares metal material surface superhydrophobic microstructure, the method utilizes femtosecond laser Radiation field induce on metallic target material surface the generation cycle be 50nm-50 μm, contact angle be 150 ° of 175 ° of different scales and The metal micro-nano structure super hydrophobic surface of pattern.The patent of Application No. 201510279045.1 discloses one kind using ultrashort The method that pulse laser prepares aluminium alloy super-hydrophobic automatic cleaning surface, the method is in pretreated aluminium alloy print surface profit Process countless micro structures with ultra-short pulse laser, put into afterwards to toast in electrically heated drying cabinet and must arrive surface there is micron order mastoid process Shape or the superhydrophobic surface of aluminum alloy of vesicular texture.The patent of Application No. 201210278261.0 discloses one kind and will clean Metallic copper workpiece immersion equipped with pure water reactor sealing after in 120 DEG C of baking ovens be incubated 1 hour, be obtained super-hydrophobic metallic copper The method on surface.The patent of Application No. 201510530848.x is disclosed one kind and is combined using chemical etching and hydrothermal treatment consists Method, in copper surface construction coarse structure, can strong adsorption stearic acid molecule, so that obtained super hydrophobic surface is had stronger Decay resistance.
The preparation method of above-described super hydrophobic surface all has the advantages that certain, but there is also some problems, such as adopts Processing cost is made to increase with femto-second laser, have is not suitable for industry to operating environment requirements harshness (need to process in vacuum environment) Metaplasia is produced;In hydro-thermal reaction, the super-hydrophobic effect that can not be obtained as reaction reagent with pure water;How using simple Method prepares stable superhydrophobic microstructure surface, and the application meeting it in industrial aspect is particularly important.
Content of the invention
The present invention is to solve femto-second laser high processing costs present in prior art, environmental requirement harshness is lacked Fall into, a kind of preparation method of pyrite super-drainage structure please be provided.
For solving above-mentioned technical problem, the technical solution adopted in the present invention is: a kind of pyrite based super hydrophobic micro structure table The preparation method in face, comprises the steps:
(1) pretreatment: Brass sample is polished, cleans and obtain Brass sample after drying;
(2) Laser Micro-Machining: laser scanning process is carried out to sample surfaces using iraser marking machine;
(3) hydrothermal treatment consists: the sample clean after Laser Micro-Machining is removed the processing spittle, then in distilled water and Methanamide Mixed liquor in put into this sample and zinc metal sheet, carry out hydrothermal treatment consists in hydrothermal reaction kettle;
(4) surface modification: the sample after hydrothermal treatment consists is placed in 1h, 1h, 2h, 2h- perfluoro decyl triethoxysilane Soak in ethanol solution, make sample surfaces row become one layer of hydrophobic film, take out and dry, that is, super hydrophobic surface is obtained.Wherein 1h, 1h, 2h, 2h- perfluoro decyl triethoxysilane can form the strong-hydrophobicity group containing-cf3 in matrix surface, improves hydrophobic Effect, and tradition is commonly used stearic acid and is formed in matrix surface and contains carboxyl hydrophobic group, but stearic acid does not dissolve at normal temperatures Water, can not be dissolved in the reagent such as ethanol under low temperature, configuration stearic acid etching liquid condition is harsher.
Preferably, the sanding operation described in step (1) is that Brass sample is sequentially passed through 400#, 1000#, 3000# Sand papering, described ultrasonic cleaning is with dehydrated alcohol and distilled water, the sample after polishing to be carried out ultrasound wave successively clean, Cleaning temperature is 40-60 DEG C, cleans 15-30min, described drying condition is that 20- is dried in 50-80 DEG C of constant temperature oven 30min.
Further, the technological parameter that the laser scanning described in step (2) is processed is that optical maser wavelength is 1064nm, maximum Laser output power is 20w, laser frequency is 20khz, the electric current density that uses is 11-14a when processing.
Preferably, in laser scanning processing procedure described in step (2) scanning speed of laser be 500-1500mm/s, The single exposure time is to be spaced apart 30-50 μm between 2-5ms, adjacent scanning lines, and scans speed in single sample processing procedure Degree, single exposure time, the interval between adjacent scanning lines all keep constant.
Preferably, the described cleaning described in step (3) is dilute hydrochloric acid, the distilled water that sample is used 1.6mol/l successively It is cleaned by ultrasonic 5~10min to remove the processing spittle under 40~60 DEG C of constant temperature.
Preferably, distilled water with the volume ratio of Methanamide is in the mixed liquor of the described distilled water of step (3) and Methanamide 20:1, described hydrothermal treatment consists temperature is 120~150 DEG C, processes 1h.
Preferably, the 1h described in step (4), 1h in the ethanol solution of 1h, 2h, 2h- perfluoro decyl triethoxysilane, 2h, 2h, 2h perfluor certain herbaceous plants with big flowers ethyl triethoxy silicane alkane mass fraction is 1%-4%.
Further, the soak time described in step (4) is 10~12h.
Preferably, the drying condition described in step (4) is that 20~30min is dried in 120 DEG C of constant temperature ovens.
Specifically, described iraser marking machine includes laser instrument and the laser beam along the output of described laser instrument is propagated The x-axis reflecting mirror in direction, y-axis reflecting mirror and f- θ lens, described x-axis reflecting mirror is driven by x-axis motor and rotates along x-axis, described y Axle reflecting mirror is driven by y-axis motor and rotates along y-axis.
Advantages of the present invention is:
1. preparation process is simple, raw material are easy to get.The method being combined using Laser Micro-Machining and hydrothermal technology, big The preparation of pyrite based super hydrophobic micro-structure surface is can achieve under compression ring border.In addition, adding zinc metal sheet, zinc in hydrothermal reaction process Piece decomposes can become zinc ion zn in formyl amine aqueous solution2+, zinc ion runs into the hydroxyl oh in water-Zn can be generated (oh)2, zn (oh)2Constantly it is deposited on brass surfaces and forms zno, separate out nanostructured after zno supersaturation so that brass surfaces There is super-hydrophobicity.
2. processing cost is low compared with femto-second laser, machined parameters are individually controllable.Can be by meter using iraser marking machine The programming of calculation machine can achieve dot matrix, straight line, the scanning of latticed micro structure;The mean power of laser, scanning speed, single expose simultaneously The technological parameters such as the interval between light time, adjacent scanning lines are individually controllable.
3. the pyrite based super hydrophobic micro-structure surface obtained by has coarse micrometer structure, to the contact angle of water about 150°.
4. the aluminium alloy pyrite based super hydrophobic micro-structure surface obtained by has good corrosion resistance, can be applicable to condense The parts such as device, water pipe, pin, it is easy to accomplish commercial Application.
Brief description
Fig. 1 laser marking machine work flow schematic diagram;
Fig. 2 laser marking machine galvanometer system schematic diagram;
Fig. 3 laser prepares the schematic flow sheet of pyrite based super hydrophobic micro-structure surface with reference to hydro-thermal method;
The pyrite substrate superhydrophobic surface micro-structure diagram that Fig. 4 iraser marking machine prepares;
The contact angle schematic diagram of the pyrite substrate superhydrophobic surface that Fig. 5 iraser marking machine prepares;
Wherein 1. computers, 2. laser instrument, 3. laser beam, 4.x spindle motor, 5.x axle reflecting mirror, 6.y spindle motor, 7.f- θ Lens, 8.y axle reflecting mirror.
Specific embodiment
Fig. 1 is laser marking machine work flow schematic diagram.First pass through host computer man-machine interactive system to Laser Processing ginseng Number is configured generating marking data;Then marking data is transferred on controller, on the one hand controller controls laser instrument, root The energy density of laser is set according to marking data;On the other hand control galvanometer scanning system, the laser that laser instrument sends is passed through Motor operation in galvanometer system controls the propagation path of laser, realizes high accuracy mark.
Fig. 2 is laser marking machine galvanometer scanning system schematic diagram.Laser processing parameter is arranged by computer 1, controls and swash Light device 2 outgoing laser beam 3, laser beam is incided on x-axis reflecting mirror 5 and y-axis reflecting mirror 8, is controlled respectively using computer 1 simultaneously X-axis motor 4 processed and y-axis motor 6 operate, and drive x-axis reflecting mirror 5 and y-axis reflecting mirror 8 to rotate along x, y-axis respectively, saturating by f- θ Mirror 7 is fallen on workpiece after focusing on some collimated light beam, thus realizing laser marking.
Fig. 3 prepares the schematic flow sheet of pyrite based super hydrophobic micro-structure surface for laser with reference to hydro-thermal method.First by pyrite Sample surfaces sanding, and polished surface is cleaned by ultrasonic to remove surface impurity;Then iraser marking machine is used to pass through setting Related technological parameter, carries out the micro structure processing of sample surfaces;Then sample is put into the water preparing correlated response reagent In thermal response kettle, under high temperature, carry out hydro-thermal reaction;Finally pass through silanization treatment at room temperature, obtain superhydrophobic microstructure table Face.
In order to be better understood from the present invention, below in conjunction with instantiation, technical scheme is done further details of Introduce.Described in following embodiments, experimental technique is conventional method if no special instructions, and described reagent and material are such as no special Illustrate all can obtain from commercial channels.
Embodiment 1
A kind of preparation method of pyrite based super hydrophobic micro-structure surface of the present embodiment, comprises the steps:
(1) pretreatment: by h62 pyrite print successively through 400#、1000#、3000#Sand papering, the sample after grinding process Product carry out ultrasound wave with dehydrated alcohol and distilled water successively and clean, and ultrasonic temperature is 40~60 DEG C, and the time is 20min, then 50 30min is dried in~80 DEG C of constant temperature ovens, obtains the Brass sample of cleaning;
(2) Laser Micro-Machining: sample surfaces are swashed using the technological parameter that iraser marking machine regulates correlation Photoscanning is processed;The wavelength of laser be 1064nm, maximum laser output be 16w, laser frequency be 20khz, processing when make Electric current density is 13a, laser aperture is 80 μm, is between 2ms, adjacent scanning lines using dot matrix processing single time of exposure Be spaced apart 50 μm;
(3) hydrothermal treatment consists: the sample after Laser Processing is put in ultrasonic washing unit and uses that 1.6mol/l's is dilute successively Hydrochloric acid, distilled water are cleaned by ultrasonic 10min to remove the processing spittle under 40~60 DEG C of constant temperature, put into the distillation of 20ml in beaker The formamide solution magnetic agitation of water and 1ml is uniformly fallen back in thermal response kettle inner bag, and vertically puts into latten(-tin) and zinc metal sheet, Inner bag is put into good seal in 50m teflon-lined hydrothermal reaction kettle, then is incubated 1 hour in 130 DEG C of constant temperature ovens;
(4) surface modification: the sample after hydrothermal treatment consists is placed in the 1h of 1%wt, 1h, 2h, 2h- perfluoro decyl triethoxy Soak 12h at room temperature in silane ethanol solution, make sample surfaces form one layer of hydrophobic film, then take out and put into 120 DEG C of perseverances 30min is dried in warm baking oven, that is, the described super hydrophobic surface with coarse structure is obtained.
The pyrite substrate superhydrophobic surface micro-structure diagram that this example is obtained is as shown in figure 4, surface is in micron order coarse structure.
The contact angle of the pyrite substrate superhydrophobic surface that this example is obtained is as shown in figure 5, be 149 ° with the contact angle of water.

Claims (10)

1. a kind of preparation method of pyrite based super hydrophobic micro-structure surface it is characterised in that: comprise the steps:
(1) pretreatment: Brass sample is polished, cleans and obtain after drying the sample of cleaning;
(2) Laser Micro-Machining: laser scanning process is carried out to sample surfaces using iraser marking machine;
(3) hydrothermal treatment consists: by the sample clean after Laser Micro-Machining removing the processing spittle, then in distilled water and Methanamide Put into this sample and zinc metal sheet in mixed liquor, carry out hydrothermal treatment consists in hydrothermal reaction kettle;
(4) surface modification: the sample after hydrothermal treatment consists is placed in 1h, the ethanol of 1h, 2h, 2h- perfluoro decyl triethoxysilane Soak in solution, make sample surfaces row become one layer of hydrophobic film, take out and dry, that is, super hydrophobic surface is obtained.
2. pyrite based super hydrophobic micro-structure surface according to claim 1 preparation method it is characterised in that: step (1) Described in sanding operation be that Brass sample is sequentially passed through 400#, 1000#, 3000# sand papering, described ultrasonic cleaning is Sample after polishing is carried out ultrasound wave with dehydrated alcohol and distilled water successively clean, cleaning temperature is 40-60 DEG C, cleaning 15-30min, described dry baking condition is that 20-30min is dried in 50-80 DEG C of constant temperature oven.
3. pyrite based super hydrophobic micro-structure surface according to claim 1 and 2 preparation method it is characterised in that: step (2) technological parameter that the laser scanning described in is processed is that optical maser wavelength is 1064nm, and maximum laser output is 20w, laser Frequency is 20khz, the electric current density that uses is 11-14a when processing.
4. pyrite based super hydrophobic micro-structure surface according to claim 3 preparation method it is characterised in that: step (2) In described laser scanning processing procedure the scanning speed of laser be 500-1500mm/s, the single exposure time be 2-5ms, adjacent It is spaced apart 30-50 μm between scan line, and scanning speed, single exposure time, adjacent scanning in single sample processing procedure Interval between line all keeps constant.
5. pyrite based super hydrophobic micro-structure surface according to claim 1 preparation method it is characterised in that: step (3) Described described cleaning is that sample is used the dilute hydrochloric acid of 1.6mol/l, distilled water are cleaned by ultrasonic successively under 40~60 DEG C of constant temperature 5~10min is to remove the processing spittle.
6. pyrite based super hydrophobic micro-structure surface according to claim 1 preparation method it is characterised in that: step (3) In the mixed liquor of described distilled water and Methanamide, distilled water and the volume ratio of Methanamide are 20:1, and described hydrothermal treatment consists temperature is 120~150 DEG C, process 1h.
7. pyrite based super hydrophobic micro-structure surface according to claim 1 preparation method it is characterised in that: step (4) Described 1h, 1h in the ethanol solution of 1h, 2h, 2h- perfluoro decyl triethoxysilane, 1h, 2h, 2h- perfluoro decyl three ethoxy Base silane mass fraction is 1%-4%.
8. pyrite based super hydrophobic micro-structure surface according to claim 7 preparation method it is characterised in that: step (4) Described soak time is 10~12h.
9. pyrite based super hydrophobic micro-structure surface according to claim 7 preparation method it is characterised in that: step (4) Described drying condition is that 20~30min is dried in 120 DEG C of constant temperature ovens.
10. pyrite based super hydrophobic micro-structure surface according to claim 1 preparation method it is characterised in that: described Iraser marking machine includes laser instrument and the x-axis reflecting mirror of the laser beam direction of propagation exporting along described laser instrument, y-axis are anti- Penetrate mirror and f- θ lens, described x-axis reflecting mirror is driven by x-axis motor and rotates along x-axis, described y-axis reflecting mirror is driven by y-axis motor Rotate along y-axis.
CN201611094585.3A 2016-12-02 2016-12-02 Method for preparing brass-based super-hydrophobic microstructural surface Pending CN106367739A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611094585.3A CN106367739A (en) 2016-12-02 2016-12-02 Method for preparing brass-based super-hydrophobic microstructural surface

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611094585.3A CN106367739A (en) 2016-12-02 2016-12-02 Method for preparing brass-based super-hydrophobic microstructural surface

Publications (1)

Publication Number Publication Date
CN106367739A true CN106367739A (en) 2017-02-01

Family

ID=57892370

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201611094585.3A Pending CN106367739A (en) 2016-12-02 2016-12-02 Method for preparing brass-based super-hydrophobic microstructural surface

Country Status (1)

Country Link
CN (1) CN106367739A (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107096998A (en) * 2017-05-08 2017-08-29 英诺激光科技股份有限公司 It is a kind of to carry out anticorrosive beating calibration method using ultrafast laser
CN107723687A (en) * 2017-09-25 2018-02-23 常州市瑞泰物资有限公司 A kind of preparation method of based superhydrophobic thin films
CN108941924A (en) * 2018-07-19 2018-12-07 江苏理工学院 A kind of method of infrared laser etch aluminum alloy microstructure function surface
CN109021826A (en) * 2018-05-15 2018-12-18 天津大学 A kind of method for preparing super-hydrophobic surface based on metal material
CN109989090A (en) * 2019-04-29 2019-07-09 江苏理工学院 A method of corrosion stability of magnesium alloy film layer is prepared using superslide surface
CN110549270A (en) * 2019-09-25 2019-12-10 天津大学 Micro gripper with bionic super-hydrophobic structure and manufacturing method of jaw end face of micro gripper
CN112095098A (en) * 2020-09-22 2020-12-18 湖北大学 Method for applying material with regular convex array and sliding surface to water mist collection
CN113278958A (en) * 2021-05-17 2021-08-20 西南交通大学 Preparation method of titanium alloy bionic super-hydrophobic surface

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104494134A (en) * 2014-12-17 2015-04-08 湖北理工学院 Method for preparing super-hydrophobic surface material with adjustable contact angle by one-step laser method
US20150208662A1 (en) * 2014-01-29 2015-07-30 Catcher Technology Co., Ltd. Antimicrobial complex surface and method of fabricating the same
CN104911599A (en) * 2015-05-28 2015-09-16 湖北工业大学 Method for preparation of aluminium alloy superhydrophobic self-cleaning surface by use of ultrafast laser
CN105521934A (en) * 2016-02-02 2016-04-27 浙江大学 Preparation method of super-hydrophobic coating layer on aluminum surface

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150208662A1 (en) * 2014-01-29 2015-07-30 Catcher Technology Co., Ltd. Antimicrobial complex surface and method of fabricating the same
CN104494134A (en) * 2014-12-17 2015-04-08 湖北理工学院 Method for preparing super-hydrophobic surface material with adjustable contact angle by one-step laser method
CN104911599A (en) * 2015-05-28 2015-09-16 湖北工业大学 Method for preparation of aluminium alloy superhydrophobic self-cleaning surface by use of ultrafast laser
CN105521934A (en) * 2016-02-02 2016-04-27 浙江大学 Preparation method of super-hydrophobic coating layer on aluminum surface

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王泽等: ""球状氧化锌薄膜的超疏水性能研究"", 《材料导报》 *
连峰等: ""超疏水钛合金表面的制备及其摩擦学性能"", 《中国有色金属学报》 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107096998A (en) * 2017-05-08 2017-08-29 英诺激光科技股份有限公司 It is a kind of to carry out anticorrosive beating calibration method using ultrafast laser
CN107723687A (en) * 2017-09-25 2018-02-23 常州市瑞泰物资有限公司 A kind of preparation method of based superhydrophobic thin films
CN109021826A (en) * 2018-05-15 2018-12-18 天津大学 A kind of method for preparing super-hydrophobic surface based on metal material
CN108941924A (en) * 2018-07-19 2018-12-07 江苏理工学院 A kind of method of infrared laser etch aluminum alloy microstructure function surface
CN109989090A (en) * 2019-04-29 2019-07-09 江苏理工学院 A method of corrosion stability of magnesium alloy film layer is prepared using superslide surface
CN110549270A (en) * 2019-09-25 2019-12-10 天津大学 Micro gripper with bionic super-hydrophobic structure and manufacturing method of jaw end face of micro gripper
CN112095098A (en) * 2020-09-22 2020-12-18 湖北大学 Method for applying material with regular convex array and sliding surface to water mist collection
CN112095098B (en) * 2020-09-22 2021-12-17 湖北大学 Method for applying material with regular convex array and sliding surface to water mist collection
CN113278958A (en) * 2021-05-17 2021-08-20 西南交通大学 Preparation method of titanium alloy bionic super-hydrophobic surface

Similar Documents

Publication Publication Date Title
CN106367739A (en) Method for preparing brass-based super-hydrophobic microstructural surface
CN106400022A (en) Method for preparing aluminum alloy super-hydrophobic functional surface by laser marking machine
Lin et al. Durable and robust transparent superhydrophobic glass surfaces fabricated by a femtosecond laser with exceptional water repellency and thermostability
CN101219506B (en) Laser production method for metal base ultra-hydrophobicity micro-structure surface
CN110548730A (en) Laser cleaning device and method for aluminum alloy anodic oxide film and surface paint film composite layer
CN104911599B (en) A kind of method that aluminium alloy super-hydrophobic automatic cleaning surface is prepared using ultrafast laser
CN104985328B (en) A kind of method that utilization nanosecond laser prepares titanium alloy super-hydrophobic frost resistance surface
CN108941924A (en) A kind of method of infrared laser etch aluminum alloy microstructure function surface
CN106583930A (en) Method for achieving reversible wettability of titanium sheet based on femtosecond laser direct writing
CN108356409A (en) A kind of underwater bubble tuning titanium sheet and its processing method and application method
CN104907697B (en) A kind of method that utilization ultrafast laser prepares titanium alloy super-hydrophobic frost resistance surface
CN109954966A (en) The method for carrying out Treatment of Metal Surface by femtosecond laser
CN109128512B (en) Micro-nano self-organizing structure prepared on surface of stainless steel and preparation method
CN109226098A (en) A kind of laser cleaning original position electric deposition device and method
CN111805089A (en) Stable super-hydrophobic self-cleaning surface and preparation method thereof by double-beam interference method
CN107740148A (en) It is a kind of in the without polishing quick method for preparing bionic super-hydrophobic surface of copper-based surfaces
CN109249137A (en) A kind of method of laser and the compound etching super-hydrophobic aluminum alloy surface of aqueous slkali
CN107500554A (en) A kind of super-hydrophobic transparent glass and preparation method thereof
CN110449418A (en) A kind of surface paint removal method and its application of Aluminum alloy airplane skin
CN109483058A (en) A method of rapid large-area remotely prepares super-hydrophobic antireflex structure on irregular metal curved surface
Cheng et al. Anti-reflective and anticorrosive properties of laser-etched titanium sheet in different media
CN107812678A (en) A kind of method that floride-free super-hydrophobic surface is prepared on metal
CN104911600B (en) A kind of method that utilization short-pulse laser prepares brass super-hydrophobic automatic cleaning surface
Li et al. Removal mechanisms and microstructure characteristics of laser paint stripping on aircraft skin surface
CN208643532U (en) A kind of aluminium alloy anode oxide film dry laser cleaning equipment

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20170201